CN101362084B - Visible-light response nano Bi3NbO7 photocatalyst preparation method and use thereof - Google Patents

Visible-light response nano Bi3NbO7 photocatalyst preparation method and use thereof Download PDF

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CN101362084B
CN101362084B CN2008101970230A CN200810197023A CN101362084B CN 101362084 B CN101362084 B CN 101362084B CN 2008101970230 A CN2008101970230 A CN 2008101970230A CN 200810197023 A CN200810197023 A CN 200810197023A CN 101362084 B CN101362084 B CN 101362084B
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water
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CN101362084A (en
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张高科
杨军玲
李名
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 Bi3NbO7, and the application of the Bi3NbO7. The preparation method comprises the following steps: Nb2O5 is taken as raw material to prepare a hydrosoluble niobium oxalate aqueous solution by a hydrothermal method; 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 an aqueous solution of bismuth; then, the niobium oxalate aqueous solution is added into the aqueous solution of bismuth according to the composition of a mixture ratio, and the obtained solution is heated and stirred under 60 DEG C to 80 DEG C so as to obtain a precursor solution of Bi3NbO7 photocatalyst which is then treated with polyesterification and is burnedto decarburize and then roasted under 450 DEG C to 750 DEG C to obtain the nanometer Bi3NbO7 photocatalyst. The activity of the nanometer Bi3NbO7 photocatalyst prepared by the invention is far higherthan that prepared by the traditional solid phase method and the preparation method is characterized by low synthesis temperature and simple and convenient operation.

Description

Visible-light response nano Bi 3NbO 7The preparation method of photochemical catalyst and application thereof
Technical field
The present invention relates to Bi 3NbO 7Preparation method and Bi 3NbO 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; usually be mixed with dephasign, 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 visible light catalysis activity 3NbO 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 3NbO 7The preparation method of photochemical catalyst is characterized in that it comprises the steps:
1) presses Nb 2O 5With the proportioning of KOH solution be 1～3g: 60～80ml, choose Nb 2O 5With KOH solution, standby; Wherein the concentration of KOH solution is 2～4mol/L;
With Nb 2O 5Put in the KOH solution, heated sealed forms water white solution in the reactor under 160～200 ℃ of environment, and under stirring condition, dripping hydrochloric acid transfers to 4～6 with pH value of solution, makes niobium in the solution fully with niobic acid (Nb 2O 5NH 2O) form is precipitated out, and gets sediment; Potassium ion with the remnants that adsorb on the deionized water rinsing removal sediment obtains the niobic acid sediment;
2) the niobic acid sediment that obtains is added oxalic acid, under 60～80 ℃ of heating conditions, constantly stir, promptly obtain the water miscible niobium oxalate aqueous solution; Wherein the quality proportioning of niobic acid sediment and oxalic acid is 1: 10～25;
3) mol ratio by niobium in the niobium oxalate aqueous solution and five water bismuth nitrates is 1: 3, chooses the niobium 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: 4～1: 6, chooses citric acid; Mol ratio by Bi in the five water bismuth nitrates and chelating agent EDTA (ethylenediamine tetra-acetic acid) is 1: 2～1: 5, chooses chelating agent EDTA (ethylenediamine tetra-acetic acid), and is standby; Proportioning by chelating agent EDTA and ammoniacal liquor is 23～27g: 100ml, chooses ammoniacal liquor;
Five water bismuth nitrates are joined in the citric acid solution of 0.4～0.6mol/L and stir down, add the mixed solution of chelating agent EDTA and ammoniacal liquor, dissolve the solution of the water white bismuth of formation until five water bismuth nitrates fully at 60～80 ℃;
The niobium oxalate aqueous solution is joined in the solution of bismuth, added thermal agitation 2～4 hours, obtain black resins viscosity, many bubbles at 60～80 ℃; Be heated to 100～200 ℃ of gels 2～4 hours then, obtain colloidal polymer;
4) with above-mentioned colloidal polymer in 300～450 ℃ of calcination 2～4h, promptly obtain Bi 3NbO 7The presoma of photochemical catalyst; With Bi 3NbO 7After the presoma of photochemical catalyst grinds,, get visible-light response nano Bi at 450～750 ℃ of calcination 4～6h 3NbO 7Photochemical catalyst.
Described visible-light response nano Bi 3NbO 7Photochemical catalyst has cubic structure, and its crystallite dimension is in 5～80 nanometers.
Described visible-light response nano Bi 3NbO 7The application of photochemical catalyst is characterized in that it is as photocatalyst applications.This photochemical catalyst (under the λ 〉=420nm), has good photocatalytic activity at visible light.
The invention has the beneficial effects as follows: use Nb 2O 5Be raw material, obtained the water miscible niobium oxalate aqueous solution by hydrothermal method, again by citric acid method under lower synthesis temperature (450～750 ℃), obtained the much higher nanometer Bi of specific activity conventional solid-state method 3NbO 7Photochemical catalyst, the nanometer Bi of acquisition 3NbO 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 3NbO 7The preparation method of photochemical catalyst, it comprises the steps:
1) takes by weighing the Nb of 2.0000g 2O 5Joining 70ml concentration is in the KOH solution of 3mol/L, and heated sealed forms water white solution in the reactor of the polytetrafluoroethylene (PTFE) under 200 ℃ of environment, under stirring condition, adds HCl solution and regulates pH to 5, makes niobium in the solution fully with niobic acid (Nb 2O 5NH 2O) form is precipitated out, and obtains white precipitate, washes precipitation repeatedly 3～5 times with distilled water, to remove the potassium ion that precipitation goes up absorption, obtains the niobic acid sediment;
2) the niobic acid sediment that obtains is added 20 oxalic acid that restrain (this moment, the quality proportioning of niobic acid sediment and oxalic acid was about 1: 10), under 80 ℃ of heating conditions and constantly, stir, promptly obtain the water miscible niobium oxalate aqueous solution (being the oxalates aqueous solution of niobium);
3) getting 0.15mol[is 31.521g] citric acid adds in the 300ml deionized water, adding 0.03mol[again is 14.5521g] Bi (NO 3) 35H 2O places 80 ℃ of stirring in water bath, gets solution A; Getting 0.09mol[is 26.3025g] chelating agent EDTA is dissolved in the 100ml concentrated ammonia liquor, adds in the above-mentioned solution A again, dissolves the solution that forms water white bismuth fully until five water bismuth nitrates; Again the 0.01mol niobium oxalate aqueous solution is added in the solution of above-mentioned bismuth, stirred 3 hours down in 80 ℃ again, (generate black resins viscosity, many bubbles this moment) when moisture content will evaporate to dryness in solution,, obtain colloidal polymer (thick, black) in 200 ℃ of heating gels 2 hours;
4) with above-mentioned colloidal polymer 450 ℃ of following ashing 4h in muffle furnace, promptly obtain Bi 3NbO 7The presoma of photochemical catalyst; With Bi 3NbO 7After the presoma of photochemical catalyst grinds,, get visible-light response nano Bi at 550 ℃ of calcination 6h 3NbO 7Photochemical catalyst.
The visible-light response nano Bi that this embodiment synthesizes 3NbO 7Photochemical catalyst, it consists of compd B i 3NbO 7, the crystallite dimension of this compound is in 15～60 nanometers.Visible-light response nano Bi 3NbO 7Photochemical catalyst is as photocatalyst applications, and in the experiment of degraded Acid Red G, dosage is 1g/L, and the concentration of Acid Red G is 50mg/L, λ 〉=420nm, and its degradation rate of 2 hours promptly reaches about 74%.
Embodiment 2:
Visible-light response nano Bi 3NbO 7The preparation method of photochemical catalyst, it comprises the steps:
1) takes by weighing the Nb of 2.0000g 2O 5Joining 70ml concentration is in the KOH solution of 3mol/L, and heated sealed forms water white solution in the reactor of the polytetrafluoroethylene (PTFE) under 200 ℃ of environment, under stirring condition, drips HCl solution and regulates pH to 6, makes niobium in the solution fully with niobic acid (Nb 2O 5NH 2O) form is precipitated out, and obtains white precipitate, precipitates 3～5 times with distilled water flushing, to remove the potassium ion that precipitation goes up absorption, obtains the niobic acid sediment;
2) the niobic acid sediment that obtains is added 20 oxalic acid that restrain (this moment, the quality proportioning of niobic acid sediment and oxalic acid was 1: 10), constantly stir, promptly obtain the water miscible niobium oxalate aqueous solution (being the oxalates aqueous solution of niobium) in 80 ℃;
3) getting 0.18mol[is 37.82552g] citric acid adds in the 300ml deionized water, adding 0.03mol[again is 14.5521g] Bi (NO 3) 35H2O places stirring in water bath, gets solution A; Getting 0.08mol[is 23.3800g] chelating agent EDTA is dissolved in the 100ml concentrated ammonia liquor and adds in the above-mentioned solution A, dissolves the solution that forms water white bismuth fully until five water bismuth nitrates; Again the 0.01mol niobium oxalate aqueous solution is added in the solution of above-mentioned bismuth, stirred 3 hours down in 80 ℃ again, (generate black resins viscosity, many bubbles this moment) when moisture content will evaporate to dryness in solution, in 100 ℃ of gels 3 hours, colloid polymerization (thick, black);
4) with above-mentioned colloidal polymer in 450 ℃ of calcination 4h, promptly obtain Bi 3NbO 7The presoma of photochemical catalyst; With Bi 3NbO 7After the presoma of photochemical catalyst grinds,, get visible-light response nano Bi at 500 ℃ of calcination 6h 3NbO 7Photochemical catalyst.
The visible-light response nano Bi that this embodiment synthesizes 3NbO 7Photochemical catalyst, it consists of compd B i 3NbO 7, the crystallite dimension of this compound is in 15～60 nanometers.Visible-light response nano Bi 3NbO 7Photochemical catalyst is as photocatalyst applications, and in the experiment of degraded Acid Red G, dosage is 1g/L, and the concentration of Acid Red G is 50mg/L, λ 〉=420nm, and its degradation rate of 2 hours promptly reaches about 73%.
Embodiment 3:
Visible-light response nano Bi 3NbO 7The preparation method of photochemical catalyst, it comprises the steps:
1) presses Nb 2O 5With the proportioning of KOH solution be 1g: 60ml, choose Nb 2O 5With KOH solution, standby; Wherein the concentration of KOH solution is 2mol/L;
With Nb 2O 5Put in the KOH solution, heated sealed forms water white solution in the reactor under 160 ℃ of environment, and under stirring condition, dripping hydrochloric acid transfers to 4 with pH value of solution, makes niobium in the solution fully with niobic acid (Nb 2O 5NH 2O) form is precipitated out, and gets sediment; Potassium ion with the remnants that adsorb on the deionized water rinsing removal sediment obtains the niobic acid sediment;
2) the niobic acid sediment that obtains is added oxalic acid, under 60 ℃ of heating conditions and constantly, stir, promptly obtain the water miscible niobium oxalate aqueous solution (being the oxalates aqueous solution of niobium); Wherein the quality proportioning of niobic acid sediment and oxalic acid is 1: 10;
3) press niobium and five water bismuth nitrate (Bi (NO in the niobium oxalate aqueous solution 3) 35H 2O) mol ratio is 1: 3, chooses the niobium 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: 4, chooses citric acid; Mol ratio by Bi in the five water bismuth nitrates and chelating agent EDTA is 1: 2, chooses chelating agent EDTA, and is standby; Proportioning by chelating agent EDTA and ammoniacal liquor is 23g: 100ml, chooses ammoniacal liquor;
Five water bismuth nitrates are joined in the citric acid solution of 0.4mol/L and stir down, add the mixed solution of chelating agent EDTA and ammoniacal liquor, dissolve the solution of the water white bismuth of formation until five water bismuth nitrates fully at 60 ℃;
The niobium oxalate aqueous solution is joined in the solution of bismuth, added thermal agitation 2 hours, until generating black resins viscosity, many bubbles at 60 ℃; Be heated to 100 ℃ of gels 2 hours, until producing colloidal polymer;
4) with above-mentioned colloidal polymer in 300 ℃ of calcination 2h, promptly obtain Bi 3NbO 7The presoma of photochemical catalyst; With Bi 3NbO 7After the presoma of photochemical catalyst grinds,, get visible-light response nano Bi at 450 ℃ of calcination 4h 3NbO 7Photochemical catalyst.The visible-light response nano Bi of gained 3NbO 7Photochemical catalyst has cubic structure, and its crystallite dimension is in 5～80 nanometers.
Described visible-light response nano Bi 3NbO 7Photochemical catalyst as photocatalyst applications.
Embodiment 4:
Visible-light response nano Bi 3NbO 7The preparation method of photochemical catalyst, it comprises the steps:
1) presses Nb 2O 5With the proportioning of KOH solution be 3g: 80ml, choose Nb 2O 5With KOH solution, standby; Wherein the concentration of KOH solution is 4mol/L;
With Nb 2O 5Put in the KOH solution, heated sealed forms water white solution in the reactor under 200 ℃ of environment, and under stirring condition, dripping hydrochloric acid transfers to 6 with pH value of solution, makes niobium in the solution fully with niobic acid (Nb 2O 5NH 2O) form is precipitated out, and gets sediment; Potassium ion with the remnants that adsorb on the deionized water rinsing removal sediment obtains the niobic acid sediment;
2) the niobic acid sediment that obtains is added oxalic acid, under 80 ℃ of heating conditions and constantly, stir, promptly obtain the water miscible niobium oxalate aqueous solution (being the oxalates aqueous solution of niobium); Wherein the quality proportioning of niobic acid sediment and oxalic acid is 1: 25;
3) press niobium and five water bismuth nitrate (Bi (NO in the niobium oxalate aqueous solution 3) 35H 2O) mol ratio is 1: 3, chooses the niobium 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: 5, chooses chelating agent EDTA, and is standby; Proportioning by chelating agent EDTA and ammoniacal liquor is 27g: 100ml, chooses ammoniacal liquor;
Five water bismuth nitrates are joined in the citric acid solution of 0.6mol/L and stir down, add the mixed solution of chelating agent EDTA and ammoniacal liquor, dissolve the solution of the water white bismuth of formation until five water bismuth nitrates fully at 80 ℃;
The niobium oxalate aqueous solution is joined in the solution of bismuth, added thermal agitation 4 hours, until generating black resins viscosity, many bubbles at 80 ℃; Be heated to 200 ℃ of gels 4 hours, until producing colloidal polymer;
4) with above-mentioned colloidal polymer in 450 ℃ of calcination 4h, promptly obtain Bi 3NbO 7The presoma of photochemical catalyst; With Bi 3NbO 7After the presoma of photochemical catalyst grinds,, get visible-light response nano Bi at 750 ℃ of calcination 6h 3NbO 7Photochemical catalyst.The visible-light response nano Bi of gained 3NbO 7Photochemical catalyst has cubic structure, and its crystallite dimension is in 5～80 nanometers.
Described visible-light response nano Bi 3NbO 7Photochemical catalyst is as photocatalyst applications.

Claims (2)

1. visible-light response nano Bi 3NbO 7The preparation method of photochemical catalyst is characterized in that it comprises the steps:
1) presses Nb 2O 5With the proportioning of KOH solution be 1～3g: 60～80ml, choose Nb 2O 5With KOH solution, standby; Wherein the concentration of KOH solution is 2～4mol/L;
With Nb 2O 5Put in the KOH solution, heated sealed forms water white solution in the reactor under 160～200 ℃ of environment, and under stirring condition, dripping hydrochloric acid transfers to 4～6 with pH value of solution, makes niobium in the solution fully with niobic acid (Nb 2O 5NH 2O) form is precipitated out, and gets sediment; Potassium ion with the remnants that adsorb on the deionized water rinsing removal sediment obtains the niobic acid sediment;
2) the niobic acid sediment that obtains is added oxalic acid, under 60～80 ℃ of heating conditions, constantly stir, promptly obtain the water miscible niobium oxalate aqueous solution; Wherein the quality proportioning of niobic acid sediment and oxalic acid is 1: 10～25;
3) mol ratio by niobium in the niobium oxalate aqueous solution and five water bismuth nitrates is 1: 3, chooses the niobium 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: 4～1: 6, chooses citric acid; Mol ratio by Bi in the five water bismuth nitrates and chelating agent ethylenediamine tetra-acetic acid is 1: 2～1: 5, chooses the chelating agent ethylenediamine tetra-acetic acid, and is standby; Proportioning by chelating agent ethylenediamine tetra-acetic acid and ammoniacal liquor is 23～27g: 100ml, chooses ammoniacal liquor;
Five water bismuth nitrates are joined in the citric acid solution of 0.4～0.6mol/L and stir down, add the mixed solution of chelating agent ethylenediamine tetra-acetic acid and ammoniacal liquor, dissolve the solution of the water white bismuth of formation until five water bismuth nitrates fully at 60～80 ℃;
The niobium oxalate aqueous solution is joined in the solution of bismuth, added thermal agitation 2～4 hours, obtain black resins viscosity, many bubbles at 60～80 ℃; Be heated to 100～200 ℃ of gels 2～4 hours then, obtain colloidal polymer;
4) with above-mentioned colloidal polymer in 300～450 ℃ of calcination 2～4h, promptly obtain Bi 3NbO 7The presoma of photochemical catalyst; With Bi 3NbO 7After the presoma of photochemical catalyst grinds,, get visible-light response nano Bi at 450～750 ℃ of calcination 4～6h 3NbO 7Photochemical catalyst.
2. as the resulting visible-light response nano Bi of claim 1 3NbO 7The application of photochemical catalyst is characterized in that it is as photocatalyst applications.
CN2008101970230A 2008-09-18 2008-09-18 Visible-light response nano Bi3NbO7 photocatalyst preparation method and use thereof Expired - Fee Related CN101362084B (en)

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