CN103157498A - Synthesis method of phosphoric acid bridged and compounded TiO2-BiVO4 nanometer photocatalyst - Google Patents
Synthesis method of phosphoric acid bridged and compounded TiO2-BiVO4 nanometer photocatalyst Download PDFInfo
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Abstract
The invention relates to a synthesis method of a phosphoric acid bridged and compounded TiO2-BiVO4 nanometer photocatalyst, and particularly relates to a synthesis method of a photocatalyst and the method is used for solving the technical problem of poor activity for decomposing bismuth vanadate under irradiation of visible light to produce hydrogen in water. The method comprises the following steps of: firstly, preparing phosphoric acid modified bismuth vanadate; secondly, preparing a solution A; thirdly, preparing a solution B; fourthly, preparing titanium dioxide compound phosphoric acid bridged bismuth vanadate; and fifthly, dispersing the titanium dioxide compound phosphoric acid bridged bismuth vanadate into distilled water, adding chloroplatinic acid, stirring under the irradiation of a xenon lamp with the power of 300w, cleaning, drying and grinding to obtain the phosphoric acid bridged and compounded TiO2-BiVO4 nanometer photocatalyst. Compared with pure bismuth vanadate, the phosphoric acid bridged and compounded TiO2-BiVO4 nanometer photocatalyst provided by the invention has the advantages that the service life of a carrier of the phosphoric acid bridged and compounded TiO2-BiVO4 nanometer photocatalyst is prolonged by 1ms, and the separation efficiency of the carrier is increased by 1.5 times. The phosphoric acid bridged and compounded TiO2-BiVO4 nanometer photocatalyst has high activity for decomposing under the irradiation of the visible light to produce the hydrogen in water.
Description
Technical field
The present invention relates to a kind of synthetic method of photochemical catalyst.
Background technology
Hydrogen Energy and solar energy be all the cleaning, regenerative resource.Utilize photochemical catalyst hydrogen production by water decomposition under the irradiation of sunshine, can convert solar energy into the Hydrogen Energy of high-energy-density.In numerous visible light semiconductor catalysts, characteristics gain great popularity pucherite because its stable in properties, spectral absorption scope be large and cheap and easy to get etc.Pucherite valence band and conduction band position are all lower, and therefore under optical excitation, the hole of generation has stronger oxidability, but the electron reduction ability that produces is relatively poor.The reducing power of light induced electron and life-span thereof are the key factors that affects its light hydrogen production by water decomposition efficient.The light induced electron reducing power is poor, and itself and hydrionic reactivity are poor, have determined that the efficient of its hydrogen production by water decomposition is low.In addition, light induced electron and hydrogen ion respond are poor, make it easily compound with photohole, and the shortening electron lifetime has further affected the efficient of its hydrogen manufacturing.Yet there are no the report that utilizes hydrogen production by water decomposition under the pucherite visible light.Therefore, synthesize the pucherite with long electron lifetime with the sub-reducing power of forceful electric power catalyst based, improve the activity of catalytic decomposition water hydrogen manufacturing under its visible light condition, significant to visible light semiconductor catalyzing manufacturing of hydrogen technology.
Summary of the invention
The objective of the invention is in order to solve the technical problem of hydrogen production by water decomposition poor activity under the pucherite radiation of visible light, provide a kind of phosphoric acid bridging compound TiO
2-BiVO
4The synthetic method of nano-photocatalyst.
The TiO that the phosphoric acid bridging is compound
2-BiVO
4The synthetic method of nano-photocatalyst is carried out according to following steps:
One, the 1g pucherite is distributed in the phosphate aqueous solution that concentration is 0.001~0.01mol/L, then stirs evaporate to dryness under the condition of 80 ℃ of heating water baths, grind, at 450 ℃ of roasting 0.5h, grind, obtain the pucherite that phosphoric acid is modified;
Two, the pucherite of resulting phosphoric acid in step 1 being modified is distributed in the mixed solution that is comprised of 20ml ethanol and 5ml distilled water, splashes into 0.5~2ml mass concentration and be 65% nitric acid under stirring condition, and stirring 0.5h obtains solution A;
Three, 0.01~0.1ml butyl titanate is distributed in the 2ml absolute ethyl alcohol, stirs 30min, obtain solution B;
Four, the solution B that step 3 is obtained is added drop-wise in the solution A that step 2 obtains with the speed of 3~4 drops/secs under stirring condition, stirs 0.5h, dries under the condition of 60~100 ℃, grind, at 450 ℃ of roasting 0.5h, grind again, obtain the pucherite of the compound phosphoric acid bridging of titanium dioxide;
The pucherite of the phosphoric acid bridging that the titanium dioxide that five, step 4 is obtained is compound is distributed in 100ml distilled water, add 0.1~1ml chloroplatinic acid, be to stir 0.5h under 300w xenon lamp (filtering ultraviolet light with the 420nm optical filter) irradiation at power, washing, dry under the condition of 80 ℃, grind, namely get the compound TiO of phosphoric acid bridging
2-BiVO
4Nano-photocatalyst.
The compound TiO of phosphoric acid bridging that adopts the present invention to obtain
2-BiVO
4The nano-photocatalyst hydrogen production by water decomposition carries out according to the following steps: adopt the spherical xenon lamp of 300W as radiation source (filtering ultraviolet light with the 420nm optical filter), be placed in airtight quartz glass reactor with the pucherite of 100ml methanol aqueous solution (mass concentration is 20%) and the bridging of 0.1g phosphoric acid is catalyst based, be positioned over apart from xenon lamp 10cm place, reactor vacuumizes 0.5h (vacuum-0.095MPa).Keep the reaction solution equalization of concentration with magnetic agitation in course of reaction.After the reaction beginning, every 0.5h amount of substance of the hydrogen of gas chromatographic detection system generation.
The compound TiO of phosphoric acid bridging of the present invention
2-BiVO
4Nano-photocatalyst, the crystalline phase of nanometer pucherite is the monocline crystalline phase, the process such as modify, compound does not form the crystalline phase of pucherite and degree of crystallization etc. impacts, and this is mainly because phosphoric acid, titanium dioxide etc. are modified, compound amount less (lower than 5%) and heat treatment temperature lower (not higher than 450 ℃).
Than pure pucherite, the compound TiO of phosphoric acid bridging of the present invention
2-BiVO
4The carrier lifetime of nano-photocatalyst has extended 1ms, and carrier separation efficient has approximately improved 1.5 times.
The compound TiO of phosphoric acid bridging that adopts the present invention to synthesize
2-BiVO
4The hydrogen output of nano-photocatalyst visible light catalytic decomposition water 1h reaches 124 μ mol, and namely the hydrogen generation efficiency efficient that reaches hydrogen manufacturing reaches 124 μ molh
-1G
-1, and under the same terms, pure pucherite hydrogen output is almost nil.The compound TiO of phosphoric acid bridging of the present invention
2-BiVO
4Nano-photocatalyst has the activity of high visible light catalytic hydrogen production by water decomposition.
Utilize phosphoric acid as molecular bridge in the present invention, realize that pucherite is connected with the effective of titanium dioxide, and at composite catalyst area load nano platinum particle, make pucherite can be transferred on the titanium dioxide with higher conduction band position by the phosphoric acid molecules bridge at the electronics with higher-energy that produces under the radiation of visible light of shorter wavelength, and under the catalysis of platinum hydrogen production by water decomposition.Existence due to phosphoric acid molecules bridge and titanium dioxide, the high energy electron that pucherite produces can shift timely, it is moved back and also is inhibited simultaneously, avoided the compound fast of itself and photohole, extended the life-span of high energy electron, improved the separative efficiency of photogenerated charge, this is conducive to the raising of pucherite photocatalytic hydrogen production by water decomposition activity.At last, the electronics of transferring on the titanium dioxide conduction band is transferred on platinum, and the hydrogen ion reaction with in water realizes photocatalytic hydrogen production by water decomposition.The present invention synthesizes the compound TiO of phosphoric acid bridging
2-BiVO
4The method reaction condition of nano-photocatalyst is gentle, resulting catalyst performance is excellent, is fit to suitability for industrialized production.
Description of drawings
Fig. 1 is the test one compound TiO of phosphoric acid bridging that obtains
2-BiVO
4The XRD figure of nano-photocatalyst, in figure, a represents the TiO that the phosphoric acid bridging is compound
2-BiVO
4The XRD figure of nano-photocatalyst, b represent the XRD figure of pucherite;
Fig. 2 is the test one compound TiO of phosphoric acid bridging that obtains
2-BiVO
4The TS-SPV of nano-photocatalyst (transient state surface photovoltage) figure, in figure, a represents the TiO that the phosphoric acid bridging is compound
2-BiVO
4The TS-SPV figure of nano-photocatalyst, b represent the TS-SPV figure of pucherite;
Fig. 3 is the test one compound TiO of phosphoric acid bridging that obtains
2-BiVO
4Hydrogen amount of substance and the time history of nano-photocatalyst photocatalytic hydrogen production by water decomposition, in figure, a represents the TiO that the phosphoric acid bridging is compound
2-BiVO
4Hydrogen amount of substance and the time history of nano-photocatalyst photocatalytic hydrogen production by water decomposition, b represent hydrogen amount of substance and the time history of pucherite photocatalytic hydrogen production by water decomposition.
The specific embodiment
Technical solution of the present invention is not limited to the following cited specific embodiment, also comprises any combination between each specific embodiment.
The specific embodiment one: the compound TiO of phosphoric acid bridging in present embodiment
2-BiVO
4The synthetic method of nano-photocatalyst is carried out according to following steps:
One, the 1g pucherite is distributed in the phosphate aqueous solution that concentration is 0.001~0.01mol/L, then stirs evaporate to dryness under the condition of 80 ℃ of heating water baths, grind, at 450 ℃ of roasting 0.5h, grind, obtain the pucherite that phosphoric acid is modified;
Two, the pucherite of resulting phosphoric acid in step 1 being modified is distributed in the mixed solution that is comprised of 20ml ethanol and 5ml distilled water, splashes into 0.5~2ml mass concentration and be 65% nitric acid under stirring condition, and stirring 0.5h obtains solution A;
Three, 0.01~0.1ml butyl titanate is distributed in the 2ml absolute ethyl alcohol, stirs 30min, obtain solution B;
Four, the solution B that step 3 is obtained is added drop-wise in the solution A that step 2 obtains with the speed of 3~4 drops/secs under stirring condition, stirs 0.5h, dries under the condition of 60~100 ℃, grind, at 450 ℃ of roasting 0.5h, grind again, obtain the pucherite of the compound phosphoric acid bridging of titanium dioxide;
The pucherite of the phosphoric acid bridging that the titanium dioxide that five, step 4 is obtained is compound is distributed in 100ml distilled water, add 0.1~1ml chloroplatinic acid, be to stir 0.5h under 300w xenon lamp (filtering ultraviolet light with the 420nm optical filter) irradiation at power, washing, dry under the condition of 80 ℃, grind, namely get the compound TiO of phosphoric acid bridging
2-BiVO
4Nano-photocatalyst.
The compound TiO of phosphoric acid bridging that obtains in present embodiment
2-BiVO
4The efficient that nano-photocatalyst is hydrogen production by water decomposition in 20% methanol aqueous solution in mass concentration reaches 124 μ molh
-1G
-1
The specific embodiment two: present embodiment is different from the specific embodiment one is that the concentration of phosphate aqueous solution in step 1 is 0.002~0.009mol/L.Other is identical with the specific embodiment one.
The specific embodiment three: present embodiment is different from one of the specific embodiment one or two is that the concentration of phosphate aqueous solution in step 1 is 0.003~0.008mol/L.Other is not identical with one of the specific embodiment one or two.
The specific embodiment four: present embodiment is different from one of specific embodiment one to three is that the concentration of phosphate aqueous solution in step 1 is 0.005mol/L.Other is identical with one of specific embodiment one to three.
The specific embodiment five: present embodiment is different from one of specific embodiment one to four is that to splash into the 1ml mass concentration in step 2 be 65% nitric acid.Other is identical with one of specific embodiment one to four.
The specific embodiment six: present embodiment is different from one of specific embodiment one to five is that to splash into the 1.5ml mass concentration in step 2 be 65% nitric acid.Other is identical with one of specific embodiment one to five.
The specific embodiment seven: what present embodiment was different from one of specific embodiment one to six is in step 3,0.02~0.09ml butyl titanate to be distributed in the 2ml absolute ethyl alcohol.Other is identical with one of specific embodiment one to six.
The specific embodiment eight: what present embodiment was different from one of specific embodiment one to seven is in step 3, the 0.05ml butyl titanate to be distributed in the 2ml absolute ethyl alcohol.Other is identical with one of specific embodiment one to seven.
The specific embodiment nine: what present embodiment was different from one of specific embodiment one to eight is to dry under the condition of 80 ℃ in step 4.Other is identical with one of specific embodiment one to eight.
The specific embodiment ten: what present embodiment was different from one of specific embodiment one to nine is to add the 0.5ml chloroplatinic acid in step 5.Other is identical with one of specific embodiment one to nine.
Adopt following verification experimental verification effect of the present invention:
Test one:
The TiO that the phosphoric acid bridging is compound
2-BiVO
4The synthetic method of nano-photocatalyst is carried out according to following steps:
One, the 1g pucherite is distributed in the phosphate aqueous solution that concentration is 0.005mol/L, then stirs evaporate to dryness under the condition of 80 ℃ of heating water baths, grind, at 450 ℃ of roasting 0.5h, grind, obtain the pucherite that phosphoric acid is modified;
Two, the pucherite of resulting phosphoric acid in step 1 being modified is distributed in the mixed solution that is comprised of 20ml ethanol and 5ml distilled water, splashes into the 1ml mass concentration and be 65% nitric acid under stirring condition, and stirring 0.5h obtains solution A;
Three, the 0.5ml butyl titanate is distributed in the 2ml absolute ethyl alcohol, stirs 30min, obtain solution B;
Four, the solution B that step 3 is obtained is added drop-wise in the solution A that step 2 obtains with the speed of 3 drops/secs under stirring condition, stirs 0.5h, dries under the condition of 80 ℃, grind, at 450 ℃ of roasting 0.5h, grind again, obtain the pucherite of the compound phosphoric acid bridging of titanium dioxide;
The pucherite of the phosphoric acid bridging that the titanium dioxide that five, step 4 is obtained is compound is distributed in 100ml distilled water, add the 0.5ml chloroplatinic acid, be to stir 0.5h under 300w xenon lamp (filtering ultraviolet light with the 420nm optical filter) irradiation at power, washing, dry under the condition of 80 ℃, grind, namely get the compound TiO of phosphoric acid bridging
2-BiVO
4Nano-photocatalyst.
The compound TiO of phosphoric acid bridging that obtains in this test
2-BiVO
4The XRD figure of nano-photocatalyst as shown in Figure 1, as can be seen from Figure 1, the crystalline phase of nanometer pucherite is the monocline crystalline phase, the process such as modify, compound does not form the crystalline phase of pucherite and degree of crystallization etc. impacts, and this is mainly because phosphoric acid, titanium dioxide etc. are modified, compound amount less (lower than 5%) and heat treatment temperature lower (not higher than 450 ℃).
The compound TiO of phosphoric acid bridging that obtains in this test
2-BiVO
4The TS-SPV of nano-photocatalyst (transient state surface photovoltage) schemes as shown in Figure 2, as can be seen from Figure 2, than pure pucherite, the compound TiO of phosphoric acid bridging that this test obtains
2-BiVO
4The carrier lifetime of nano-photocatalyst has extended 1ms, and carrier separation efficient has approximately improved 1.5 times.
The compound TiO of phosphoric acid bridging that adopts this test to obtain
2-BiVO
4The nano-photocatalyst hydrogen production by water decomposition carries out according to the following steps: adopt the spherical xenon lamp of 300W as radiation source (filtering ultraviolet light with the 420nm optical filter), be placed in airtight quartz glass reactor with the pucherite of 100ml methanol aqueous solution (mass concentration is 20%) and the bridging of 0.1g phosphoric acid is catalyst based, be positioned over apart from xenon lamp 10cm place, reactor vacuumizes 0.5h (vacuum-0.095MPa).Keep the reaction solution equalization of concentration with magnetic agitation in course of reaction.After the reaction beginning, every 0.5h amount of substance of the hydrogen of gas chromatographic detection system generation.
The compound TiO of phosphoric acid bridging that obtains in this test
2-BiVO
4The hydrogen amount of substance of nano-photocatalyst photocatalytic hydrogen production by water decomposition--time history as shown in Figure 3, the synthetic compound TiO of phosphoric acid bridging as can be seen from Figure 3
2-BiVO
4The hydrogen output of nano-photocatalyst visible light catalytic decomposition water 1h reaches 124 μ mol, and namely the hydrogen generation efficiency efficient that reaches hydrogen manufacturing reaches 124 μ molh
-1G
-1, and under the same terms, pure pucherite hydrogen output is almost nil.This shows the compound TiO of phosphoric acid bridging that this test obtains
2-BiVO
4Nano-photocatalyst has the activity of high visible light catalytic hydrogen production by water decomposition.
Claims (10)
1. the compound TiO of phosphoric acid bridging
2-BiVO
4The synthetic method of nano-photocatalyst is characterized in that the TiO that the phosphoric acid bridging is compound
2-BiVO
4The synthetic method of nano-photocatalyst is carried out according to following steps:
One, the 1g pucherite is distributed in the phosphate aqueous solution that concentration is 0.001~0.01mol/L, then stirs evaporate to dryness under the condition of 80 ℃ of heating water baths, grind, at 450 ℃ of roasting 0.5h, grind, obtain the pucherite that phosphoric acid is modified;
Two, the pucherite of resulting phosphoric acid in step 1 being modified is distributed in the mixed solution that is comprised of 20ml ethanol and 5ml distilled water, splashes into 0.5~2ml mass concentration and be 65% nitric acid under stirring condition, and stirring 0.5h obtains solution A;
Three, 0.01~0.1ml butyl titanate is distributed in the 2ml absolute ethyl alcohol, stirs 30min, obtain solution B;
Four, the solution B that step 3 is obtained is added drop-wise in the solution A that step 2 obtains with the speed of 3~4 drops/secs under stirring condition, stirs 0.5h, dries under the condition of 60~100 ℃, grind, at 450 ℃ of roasting 0.5h, grind again, obtain the pucherite of the compound phosphoric acid bridging of titanium dioxide;
The pucherite of the phosphoric acid bridging that the titanium dioxide that five, step 4 is obtained is compound is distributed in 100ml distilled water, adds 0.1~1ml chloroplatinic acid, stirs 0.5h under the xenon lamp that power is 300w shines, washing, dry under the condition of 80 ℃, grind, namely get the compound TiO of phosphoric acid bridging
2-BiVO
4Nano-photocatalyst.
2. the compound TiO of phosphoric acid bridging according to claim 1
2-BiVO
4The synthetic method of nano-photocatalyst, the concentration that it is characterized in that phosphate aqueous solution in step 1 is 0.002~0.009mol/L.
3. the compound TiO of phosphoric acid bridging according to claim 1
2-BiVO
4The synthetic method of nano-photocatalyst, the concentration that it is characterized in that phosphate aqueous solution in step 1 is 0.003~0.008mol/L.
4. the compound TiO of phosphoric acid bridging according to claim 1
2-BiVO
4The synthetic method of nano-photocatalyst, the concentration that it is characterized in that phosphate aqueous solution in step 1 is 0.005mol/L.
5. 2,3, the 4 or 5 compound TiO of described phosphoric acid bridging according to claim 1,
2-BiVO
4The synthetic method of nano-photocatalyst is characterized in that splashing in step 2 the 1ml mass concentration and is 65% nitric acid.
6. 2,3, the 4 or 5 compound TiO of described phosphoric acid bridging according to claim 1,
2-BiVO
4The synthetic method of nano-photocatalyst is characterized in that splashing in step 2 the 1.5ml mass concentration and is 65% nitric acid.
7. 2,3, the 4 or 5 compound TiO of described phosphoric acid bridging according to claim 1,
2-BiVO
4The synthetic method of nano-photocatalyst is characterized in that in step 3,0.02~0.09ml butyl titanate being distributed in the 2ml absolute ethyl alcohol.
8. 2,3, the 4 or 5 compound TiO of described phosphoric acid bridging according to claim 1,
2-BiVO
4The synthetic method of nano-photocatalyst is characterized in that in step 3, the 0.05ml butyl titanate being distributed in the 2ml absolute ethyl alcohol.
9. 2,3, the 4 or 5 compound TiO of described phosphoric acid bridging according to claim 1,
2-BiVO
4The synthetic method of nano-photocatalyst is characterized in that drying under the condition of 80 ℃ in step 4.
10. 2,3, the 4 or 5 compound TiO of described phosphoric acid bridging according to claim 1,
2-BiVO
4The synthetic method of nano-photocatalyst is characterized in that adding in step 5 the 0.5ml chloroplatinic acid.
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Cited By (2)
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CN103864012A (en) * | 2014-01-23 | 2014-06-18 | 燕山大学 | MgH2-BiVO4 hydrogen storage composite material and preparation method thereof |
CN105685099A (en) * | 2014-12-16 | 2016-06-22 | 昭和电工株式会社 | Method for producing BiVO4-carried titanium oxide and antiviral composition |
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CN105685099A (en) * | 2014-12-16 | 2016-06-22 | 昭和电工株式会社 | Method for producing BiVO4-carried titanium oxide and antiviral composition |
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