CN102941124A - Visible-light reaction polypyrrole/Bi2WO6 composite catalyst and preparation method thereof - Google Patents

Visible-light reaction polypyrrole/Bi2WO6 composite catalyst and preparation method thereof Download PDF

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CN102941124A
CN102941124A CN2012104721556A CN201210472155A CN102941124A CN 102941124 A CN102941124 A CN 102941124A CN 2012104721556 A CN2012104721556 A CN 2012104721556A CN 201210472155 A CN201210472155 A CN 201210472155A CN 102941124 A CN102941124 A CN 102941124A
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polypyrrole
catalyst
preparation
bi2wo6
composite photo
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CN102941124B (en
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段芳
张乾宏
魏从杰
施冬健
东为富
倪忠斌
陈明清
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Jiangnan University
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Abstract

The invention discloses a visible-light reaction polypyrrole/Bi2WO6 composite catalyst and a preparation method thereof. The visible-light reaction polypyrrole/Bi2WO6 composite catalyst is mainly characterized in that Bi2WO6 photocatalyst is easy to reunite because of photoproduction electrons-holes, photocatalytic activity of the Bi2WO6 photocatalyst is reduced, the surface of the Bi2WO6 photocatalyst is modified by conducting polymer polypyrrole, separation of the photoproduction electrons-holes can be improved remarkably, and therefore photocatalytic performance of a Bi2WO6 visible-light catalyst is improved. The preparation method includes: (1) nanometer sheet-shaped Bi2WO6 is synthetized through a hydrothermal method; and (2) the polypyrrole/Bi2WO6 composite catalyst with different polypyrrole modified quantity is obtained through in-situ polymerization. The method is simple in process and low in cost, and the prepared polypyrrole/Bi2WO6 composite catalyst has high photocatalytic activity under visual light.

Description

A kind of visible light-responded polypyrrole/Bi 2WO 6Composite catalyst and preparation method thereof
Technical field
The invention belongs to photocatalysis technology, relate to and adopt hydro-thermal method synthesis of nano sheet Bi 2WO 6, utilizing situ aggregation method, preparation conducting polymer polypyrrole is modified at laminated structure Bi 2WO 6The surface, obtain a kind of visible light-responded polypyrrole/Bi 2WO 6Composite photo-catalyst.
Background technology
The seriousness of at present environmental pollution has become one and has directly threatened human survival, needs the focal issue of solution badly.Photocatalysis technology is at the energy and environmental area the green technology of important application prospect to be arranged from what twentieth century progressively grew up the seventies.This technology can make the organic pollution generation oxidative decomposition in the environment, finally is degraded to CO 2, the small-molecule substance such as water and inorganic ions, so non-secondary pollution, the high at present the most promising pollution treatment method that is considered to of palliating degradation degree.
Bismuth based semiconductor photochemical catalyst can be had good photocatalytic activity by excited by visible light, and degradable organic pollutant has good development prospect effectively.Their common feature and significant advantage have absorption exactly in visible-range, have good photocatalysis performance.Yet bismuth based semiconductor photochemical catalyst is Bi particularly 2WO 6There is the easily again combination of light induced electron-hole in photochemical catalyst, to problems such as visible Optical Absorption limiteds, has limited greatly Bi 2WO 6The large-scale application of photochemical catalyst.Therefore, must take certain measure to improve the light induced electron transport efficiency, effectively limit again combination of electron-hole, further widen Bi 2WO 6Photochemical catalyst improves visible light-responded Bi to the absorption region of visible light 2WO 6The photocatalytic activity of photochemical catalyst.The conducting polymer polypyrrole is modified Bi 2WO 6Photochemical catalyst, electronics and hole distribution in can the change system affect the surface nature of photochemical catalyst, and then improve its photocatalytic activity.
Summary of the invention
The object of the present invention is to provide a kind of visible light-responded polypyrrole/Bi 2WO 6Composite photo-catalyst and preparation method thereof, the method technique is simple, with low cost, and synthetic composite photo-catalyst photocatalytic degradation effect is fine.
The invention provides the visible light-responded polypyrrole/Bi for degradable organic pollutant 2WO 6Composite photo-catalyst is characterized in that: the polypyrrole and the Bi that by mass ratio are 1: 1000～1: 20 2WO 6Be composited, utilize the Surface Modification Effect of conducting polymer polypyrrole, significantly improve Bi 2WO 6The visible light photocatalysis performance.Polypyrrole/Bi 2WO 6Preparation method's step of composite photo-catalyst is as follows:
(1) preparation Bi 2WO 6Precursor solution: a certain amount of bismuth salt is dissolved in the salpeter solution that concentration is 0.1～10mol/L, forms clear solution, under stirring, the tungsten salt solution that slowly adds the metering ratio, wherein the concentration of tungsten salt is controlled at 0.02～0.08mol/L, stirs 0.5～1h, obtains Bi 2WO 6Presoma suspension.
Wherein bismuth salt can be bismuth nitrate, bismuth chloride; Tungsten salt can be sodium tungstate or the villaumite that contains W.
(2) laminated structure Bi 2WO 6Preparation: with above-mentioned Bi 2WO 6Presoma suspension changes 50mL over to and contains in the teflon-lined stainless steel autoclave, and 100～240 ℃ of reaction 10～30h with the products therefrom centrifugation, and 50～100 ℃ of vacuum drying, obtain the Bi of nano-sheet structure 2WO 6Photochemical catalyst.
(3) with the laminated structure Bi of step (2) gained 2WO 6Be dispersed in deionized water for ultrasonic with neopelex and disperse to form uniform suspension, then add the pyrrole monomer of different amounts, splash at last a certain amount of FeCl 3Solution, system is blackening gradually, home position polymerization reaction 1～24h, product water and absolute ethanol washing several times after, behind 50～100 ℃ of vacuum drying 24h, obtain the polypyrrole/Bi of different polypyrrole modifying amounts 2WO 6Composite photo-catalyst.
The present invention compared with prior art has remarkable advantage:
(1) the present invention adopts hydro-thermal method synthesizing flaky structure Bi 2WO 6Photochemical catalyst, recycling polypyrrole in-situ polymerization is modified Bi 2WO 6The surface obtains polypyrrole/Bi 2WO 6Composite photo-catalyst, the method technique is simple, and is easy to operate.
(2) polypyrrole modifying of the present invention is at Bi 2WO 6Bi has significantly been widened on the surface of photochemical catalyst 2WO 6Photochemical catalyst is to the absorption region of visible light, and can make light induced electron and hole realize effectively separating, thereby significantly improves Bi 2WO 6The photochemical catalyst visible light catalysis activity.
Description of drawings
Bi before and after Fig. 1 polypyrrole modifying 2WO 6The scanning electron microscopy picture of visible light catalyst: (a) pure Bi 2WO 6, (b) polypyrrole/Bi 2WO 6Composite photo-catalyst;
Bi before and after Fig. 2 polypyrrole modifying 2WO 6The X-ray diffraction spectrogram of visible light catalyst;
Bi before and after Fig. 3 polypyrrole modifying 2WO 6Fourier's infrared spectrogram of visible light catalyst;
Bi before and after Fig. 4 polypyrrole modifying 2WO 6The UV-Vis DRS spectrum of visible light catalyst: (a) pure Bi 2WO 6, (b) polypyrrole/Bi 2WO 6Composite photo-catalyst.
The specific embodiment
Polypyrrole/Bi that the present invention is visible light-responded 2WO 6Composite photo-catalyst is 1: 1000～1: 20 polypyrrole and Bi by mass ratio 2WO 6Be composited, utilize the Surface Modification Effect of conducting polymer polypyrrole, significantly improve Bi 2WO 6The visible light photocatalysis performance.
The present invention visible light-responded polypyrrole/Bi 2WO 6The preparation method of composite photo-catalyst comprises the steps:
(1) preparation Bi 2WO 6Precursor solution: a certain amount of bismuth salt is dissolved in the salpeter solution that concentration is 0.1～10mol/L, forms clear solution, under stirring, the tungsten salt solution that slowly adds the metering ratio, wherein the concentration of tungsten salt is controlled at 0.02～0.08mol/L, stirs 0.5～1h, obtains Bi 2WO 6Presoma suspension.
Wherein bismuth salt can be bismuth nitrate, bismuth chloride; Tungsten salt can be sodium tungstate or the villaumite that contains W.
(2) laminated structure Bi 2WO 6Preparation: with above-mentioned Bi 2WO 6Presoma suspension changes 50mL over to and contains in the teflon-lined stainless steel autoclave, and 100～240 ℃ of reaction 10～30h with the products therefrom centrifugation, and 50～100 ℃ of vacuum drying, obtain the Bi of nano-sheet structure 2WO 6Photochemical catalyst.
(3) with the laminated structure Bi of step (2) gained 2WO 6Be dispersed in deionized water for ultrasonic with neopelex and disperse to form uniform suspension, then add the pyrrole monomer of different amounts, splash at last a certain amount of FeCl 3Solution, system is blackening gradually, home position polymerization reaction 1～24h, product water and absolute ethanol washing several times after, behind 60 ℃ of vacuum drying 24h, obtain the polypyrrole/Bi of different polypyrrole modifying amounts 2WO 6Composite photo-catalyst.
For a better understanding of the present invention, further illustrate content of the present invention below in conjunction with example, but content of the present invention is not limited to following given example.
The side's of enforcement example 1: a kind of visible light-responded polypyrrole/Bi of the present invention 2WO 6The preparation method of composite photo-catalyst may further comprise the steps:
(1) preparation Bi 2WO 6Precursor solution: the 2mmol bismuth nitrate is dissolved in the 2M salpeter solution, forms clear solution, under stirring, add the sodium tungstate solution 20mL of 0.05mol/L, stir 0.5h, obtain Bi 2WO 6The presoma white suspension.
(2) nano-sheet structure Bi 2WO 6Preparation: with above-mentioned Bi 2WO 6Presoma suspension changes 50mL over to and contains in the teflon-lined stainless steel autoclave, and 180 ℃ of reaction 15h naturally cool to room temperature, with the products therefrom centrifugation, and 50 ℃ of vacuum drying, obtain the Bi of nano-sheet structure 2WO 6Photochemical catalyst.
(3) get the laminated structure Bi of step (2) gained 2WO 61g and neopelex 0.2g are dispersed in the 100mL deionized water, and ultrasonic 30min obtains homodisperse suspension.Then add the 10mg pyrrole monomer, splash at last a certain amount of FeCl 3Solution, system is blackening gradually, home position polymerization reaction 12h, product water and absolute ethanol washing several times after, behind 60 ℃ of vacuum drying 24h, obtain polypyrrole/Bi 2WO 6Composite photo-catalyst.
Through SEM to Bi before and after the polypyrrole modifying 2WO 6The pattern of visible light catalyst characterizes, and its pattern has well been inherited Bi 2WO 6Laminated structure, but the surface of nanometer sheet becomes coarse, illustrates that tentatively polypyrrole is at Bi 2WO 6The surface aggregate success of laminated structure, as shown in Figure 1.To Bi before and after the polypyrrole modifying 2WO 6Phase characterize, as shown in Figure 2, Bi before and after modifying 2WO 6Phase do not change, the intensity of each diffraction maximum also not to occur significantly to change.Utilize Fourier's infrared spectrum to Bi before and after the polypyrrole modifying 2WO 6Structure test, the result shows and utilizes synthetic method of the present invention successfully to obtain polypyrrole/Bi 2WO 6Composite photo-catalyst.In addition, we utilize UV-Vis DRS spectrum to Bi before and after the polypyrrole modifying 2WO 6Absorbing state to visible light characterizes, as shown in Figure 4, and Bi behind the polypyrrole modifying 2WO 6Absorption at visible region significantly strengthens.
Embodiment 2: a kind of visible light-responded polypyrrole/Bi of the present invention 2WO 6The preparation method of composite photo-catalyst may further comprise the steps:
(1) preparation Bi 2WO 6Precursor solution: the 1mmol bismuth nitrate is dissolved in the 1M salpeter solution, forms clear solution, under stirring, add the sodium tungstate solution 10mL of 0.05mol/L, stir 0.5h, obtain Bi 2WO 6The presoma white suspension.
(2) nano-sheet structure Bi 2WO 6Preparation: with above-mentioned Bi 2WO 6Presoma suspension changes 50mL over to and contains in the teflon-lined stainless steel autoclave, and 160 ℃ of reaction 24h naturally cool to room temperature, with the products therefrom centrifugation, and 60 ℃ of vacuum drying, obtain the Bi of nano-sheet structure 2WO 6Photochemical catalyst.
(3) get the nano-sheet structure Bi of step (2) gained 2WO 61g and neopelex 0.1g are dispersed in the 100mL deionized water, and ultrasonic 30min obtains homodisperse suspension.Then add the 20mg pyrrole monomer, splash at last a certain amount of FeCl 3Solution, system is blackening gradually, home position polymerization reaction 24h, product water and absolute ethanol washing several times after, behind 60 ℃ of vacuum drying 24h, obtain polypyrrole/Bi 2WO 6Composite photo-catalyst.
Embodiment 3: a kind of visible light-responded polypyrrole/Bi of the present invention 2WO 6The preparation method of composite photo-catalyst may further comprise the steps:
(1) preparation Bi 2WO 6Precursor solution: the 2mmol bismuth nitrate is dissolved in the 1.5M salpeter solution, forms clear solution, under stirring, add the sodium tungstate solution 20mL of 0.05mol/L, stir 0.5h, obtain Bi 2WO 6The presoma white suspension.
(2) nano-sheet structure Bi 2WO 6Preparation: with above-mentioned Bi 2WO 6Presoma suspension changes 50mL over to and contains in the teflon-lined stainless steel autoclave, and 200 ℃ of reaction 12h naturally cool to room temperature, with the products therefrom centrifugation, and 60 ℃ of vacuum drying, obtain the Bi of nano-sheet structure 2WO 6Photochemical catalyst.
(3) get the nano-sheet structure Bi of step (2) gained 2WO 61g and neopelex 0.15g are dispersed in the 100mL deionized water, and ultrasonic 30min obtains homodisperse suspension.Then add the 30mg pyrrole monomer, splash at last a certain amount of FeCl 3Solution, system is blackening gradually, home position polymerization reaction 15h, product water and absolute ethanol washing several times after, behind 50 ℃ of vacuum drying 24h, obtain polypyrrole/Bi 2WO 6Composite photo-catalyst.

Claims (4)

1. visible light-responded polypyrrole/Bi 2WO 6Composite photo-catalyst is characterized in that: the polypyrrole and the Bi that by mass ratio are 1: 1000～1: 20 2WO 6Be composited, utilize the Surface Modification Effect of conducting polymer polypyrrole, significantly improve Bi 2WO 6The visible light photocatalysis performance.
2. visible light-responded polypyrrole/Bi 2WO 6The preparation method of composite photo-catalyst is characterized in that, comprises the steps:
(1) preparation Bi 2WO 6Precursor solution: a certain amount of bismuth salt is dissolved in the salpeter solution that concentration is 0.1～10mol/L, forms clear solution, under stirring, the tungsten salt solution that slowly adds the metering ratio, wherein the concentration of tungsten salt is controlled at 0.02～0.08mol/L, stirs 0.5～1h, obtains Bi 2WO 6Presoma suspension.
Wherein bismuth salt can be bismuth nitrate, bismuth chloride; Tungsten salt can be sodium tungstate or the villaumite that contains W.
(2) laminated structure Bi 2WO 6Preparation: with above-mentioned Bi 2WO 6Presoma suspension changes 50mL over to and contains in the teflon-lined stainless steel autoclave, and 100～240 ℃ of reaction 10～30h with the products therefrom centrifugation, and 50～100 ℃ of vacuum drying, obtain the Bi of nano-sheet structure 2WO 6Photochemical catalyst.
(3) with the laminated structure Bi of step (2) gained 2WO 6Be dispersed in deionized water for ultrasonic with neopelex and disperse to form uniform suspension, then add the pyrrole monomer of different amounts, splash at last a certain amount of FeCl 3Solution, system is blackening gradually, home position polymerization reaction 1～24h, product water and absolute ethanol washing several times after, behind 60 ℃ of vacuum drying 24h, obtain the polypyrrole/Bi of different polypyrrole modifying amounts 2WO 6Composite photo-catalyst.
3. polypyrrole/Bi according to claim 2 2WO 6The preparation method of composite photo-catalyst is characterized in that neopelex and Bi in the step (3) 2WO 6Mass ratio be 1: 10～1: 2.
4. polypyrrole/Bi according to claim 2 2WO 6The preparation method of composite photo-catalyst is characterized in that pyrrole monomer and Bi in the step (3) 2WO 6Mass ratio be 1: 1000～1: 20.
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CN112264092A (en) * 2020-10-19 2021-01-26 浙江大学 Polypyrrole modified TiO2Coated LaB6Preparation method of photodegradation catalyst
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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103816939A (en) * 2014-03-07 2014-05-28 青岛科技大学 Preparation method for bismuth tungstate/polyaniline heterojunction photocatalyst
CN104445420A (en) * 2014-12-09 2015-03-25 江南大学 Preparation method of bismuth tungstate photo-catalyst with vehicle wheel shaped three-dimensional hierarchical structure
CN104984764A (en) * 2015-07-08 2015-10-21 上海应用技术学院 Poly 3-hexylthiophene-Bi<2>WO<6> composite photocatalyst and preparation method thereof
CN109663615A (en) * 2018-11-30 2019-04-23 华纺股份有限公司 A kind of g-C3N4/ppy/Bi2WO6Solid-state Z-type photochemical catalyst and preparation method
CN110813376A (en) * 2019-11-13 2020-02-21 许昌学院 Polypyrrole-modified nano bismuth oxybromide photocatalytic material and preparation method and application thereof
CN112264092A (en) * 2020-10-19 2021-01-26 浙江大学 Polypyrrole modified TiO2Coated LaB6Preparation method of photodegradation catalyst
CN112169791A (en) * 2020-10-22 2021-01-05 西安理工大学 Preparation method of lamellar three-phase composite photocatalytic material
CN112169791B (en) * 2020-10-22 2022-09-02 西安理工大学 Preparation method of lamellar three-phase composite photocatalytic material
CN113231099A (en) * 2021-05-21 2021-08-10 吉林大学 Preparation and application of Z-type polypyrrole-bismuth tungstate photocatalyst

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