CN103433077A - Three-element composite photocatalyst and preparation method thereof - Google Patents
Three-element composite photocatalyst and preparation method thereof Download PDFInfo
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- CN103433077A CN103433077A CN2013104097798A CN201310409779A CN103433077A CN 103433077 A CN103433077 A CN 103433077A CN 2013104097798 A CN2013104097798 A CN 2013104097798A CN 201310409779 A CN201310409779 A CN 201310409779A CN 103433077 A CN103433077 A CN 103433077A
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Abstract
The invention discloses a three-element composite photocatalyst and a preparation method thereof, belonging to the field of photocatalysis. The invention is mainly characterized in that the synergetic effect of polyaniline, BiOCl and BiPO4 widens the spectral response range of the BiPO4 photocatalyst and increases a photogenerated electron-hole pair transfer rate, so that the photocatalyst has favorable photocatalytic property under visible light. The preparation method comprises the following steps: (1) preparation of BiPO4: dissolving a bismuth salt in a nitric acid solution with a certain concentration, adding a right amount of citric acid, mixing with stoichiometric ratio of phosphate water solution, stirring uniformly, adding into a reaction kettle, reacting, centrifuging the obtained products, and carrying out vacuum drying; and (2) taking a certain amount of BiPO4 prepared in the step (1), carrying out in-situ reaction on the BiPO4 and conductive polymer monomer aniline in hydrochloric acid with a certain concentration, washing the product with water and anhydrous ethanol for several times, and carrying out vacuum drying to obtain the polyaniline/BiOCl-modified BiPO4 three-element composite photocatalyst. The method has the advantages of simple technique and low cost; and the prepared three-element composite photocatalyst has higher visible light catalytic activity.
Description
Technical field
The invention belongs to photocatalysis technology, relate to and adopt hydro-thermal method to prepare BiPO
4particle, utilize situ aggregation method, and under the hydrochloric acid corrasion, a step has prepared the BiPO that polyaniline, BiOCl modify
4the tri compound photochemical catalyst, widened BiPO
4spectral response range, obtain having visible light-responded tri compound photochemical catalyst.
Background technology
The seriousness of environmental pollution at present, become one and directly threatened human survival, needs the focal issue of solution badly.Photocatalysis technology be from twentieth century, progressively grow up the seventies at the energy and environmental area, the green technology of important application prospect is arranged.This technology can make the organic pollution generation oxidative decomposition in environment, finally is degraded to CO
2, the small-molecule substance such as water and inorganic ions, so non-secondary pollution, the high the most promising pollution treatment method at present that is considered to of palliating degradation degree.
Bismuth based semiconductor photochemical catalyst has good photocatalytic activity, and degradable organic pollutant, have good development prospect effectively.Most of bismuth based semiconductor photochemical catalyst can, by excited by visible light, have visible light catalysis activity.Minority bismuth based semiconductor catalysis material is as BiPO
4can only under ultraviolet excitation, just there is photocatalytic activity, because ultraviolet light proportion in solar spectrum is less, limit greatly BiPO
4large-scale application.In order to make BiPO
4can under visible ray, have photocatalytic activity, it is very necessary adopting suitable means to widen its spectral response range.The design of composite photo-catalyst and preparation in recent years is the focus of photocatalysis field research, common composite photo-catalyst be take binary composition as main, wherein have and improve by heterojunction structure that light induced electron-hole separates, have and modify by surface plasma, also have by metal or nonmetallic ion-doped etc., can improve the performance of photochemical catalyst.Yet the research of tri compound photochemical catalyst is still less at present, the mutual synergy of research ternary component is very necessary on the impact of photocatalysis performance.Polyaniline, as the conducting polymer with excellent conductive performance, has remarkable absorption in visible-range, and the Surface Modification Effect by polyaniline can significantly improve BiPO
4spectral response range.In addition, although BiOCl is also the bismuth series photocatalyst of ultraviolet light response, can with BiPO
4valence band and conduction band coupling, be beneficial to separating of light induced electron and hole, can effectively change BiPO together with polyaniline
4electronics and the hole distribution on surface, affect the surface nature of photochemical catalyst, is beneficial to the separation in light induced electron-hole in photocatalytic process, the reduction electron-hole again in conjunction with probability, and then improve its photocatalytic activity.
Summary of the invention
The object of the present invention is to provide a kind of tri compound photochemical catalyst and preparation method thereof, the method technique is simple, with low cost, and synthetic composite photo-catalyst photocatalytic degradation effect is better.
The invention provides the tri compound photochemical catalyst for degradable organic pollutant, it is characterized in that: by three component polyanilines, BiOCl, BiPO
4be composited, utilize polyaniline, BiOCl and BiPO
4synergy, widened BiPO
4spectral response range, be beneficial to the separation in light induced electron-hole, make composite photo-catalyst there is the visible light catalytic performance, comprise the steps:
(1) prepare BiPO
4: a certain amount of bismuth salt is dissolved in the salpeter solution that concentration is 0.1～5mol/L, form clear solution, under stirring, slowly add 0.1～0.5mol/L citric acid solution, 5～20mL, continue to stir 0.5～1h, add again the phosphate solution that measures ratio, wherein phosphatic concentration is controlled at 0.01～0.1mol/L, stir 0.5～1h, then proceed to 50mL containing in teflon-lined stainless steel autoclave, 100～240 ℃ of reaction 10～30h, by the products therefrom centrifugation, and, 50～100 ℃ of vacuum drying, obtain BiPO
4photochemical catalyst;
(2) preparation of tri compound photochemical catalyst: get BiPO prepared by step (1)
4photochemical catalyst 0.1～0.5g adds ultrasonic dispersion in the certain density hydrochloric acid solution of 50mL, add aniline monomer under room temperature, logical nitrogen is after 20～60 minutes, add a certain amount of ammonium persulfate, room temperature reaction 0.5～10h, product is carried out to suction filtration, after water and absolute ethyl alcohol wash respectively for several times, dry in 60 ℃ of vacuum drying ovens.
The present invention compared with prior art, has remarkable advantage:
(1) the present invention adopts the auxiliary synthetic BiPO of hydro-thermal method citric acid
4photochemical catalyst, recycling aniline monomer in-situ polymerization, next step obtains the BiPO of polyaniline, BiOCl modification the hydrochloric acid corrasion
4the tri compound photochemical catalyst, the method technique is simple, easy to operate.
(2) the present invention utilizes conducting polymer polyaniline, BiOCl and BiPO
4the synergy of photochemical catalyst, significantly widened BiPO
4the spectral response range of photochemical catalyst, make it have visible light catalysis activity, and effectively increased the light induced electron of photocatalyst surface and separating of hole, thereby significantly improve BiPO
4the photocatalytic activity of photochemical catalyst, prepared tri compound photochemical catalyst photocatalytic activity is higher.
The accompanying drawing explanation
The X-ray diffraction style of Fig. 1 tri compound photochemical catalyst;
The scanning electron micrograph of Fig. 2 tri compound photochemical catalyst;
Fourier's infrared spectrogram of Fig. 3 tri compound photochemical catalyst;
The test of Fig. 4 tri compound photochemical catalyst photocatalysis performance
The specific embodiment
The invention provides the tri compound photochemical catalyst for degradable organic pollutant, it is characterized in that: by three component polyanilines, BiOCl, BiPO
4be composited, utilize polyaniline, BiOCl and BiPO
4synergy, widened BiPO
4spectral response range, be beneficial to the separation in light induced electron-hole, make composite photo-catalyst there is the visible light catalytic performance.
The preparation method of a kind of tri compound photochemical catalyst of the present invention, comprise the steps:
(1) prepare BiPO
4: a certain amount of bismuth salt is dissolved in the salpeter solution that concentration is 0.1～5mol/L, form clear solution, under stirring, slowly add 0.1～0.5mol/L citric acid solution, 5～20mL, continue to stir 0.5～1h, add again the phosphate solution that measures ratio, wherein phosphatic concentration is controlled at 0.01～0.1mol/L, stir 0.5～1h, then proceed to 50mL containing in teflon-lined stainless steel autoclave, 100～240 ℃ of reaction 10～30h, by the products therefrom centrifugation, and, 50～100 ℃ of vacuum drying, obtain BiPO
4photochemical catalyst;
(2) preparation of tri compound photochemical catalyst: get BiPO prepared by step (1)
4photochemical catalyst 0.1～0.5g adds ultrasonic dispersion in the certain density hydrochloric acid solution of 50mL, add aniline monomer under room temperature, logical nitrogen is after 20～60 minutes, add a certain amount of ammonium persulfate, room temperature reaction 0.5～10h, product is carried out to suction filtration, after water and absolute ethyl alcohol wash respectively for several times, dry in 60 ℃ of vacuum drying ovens.
For a better understanding of the present invention, below in conjunction with example, further illustrate content of the present invention, but content of the present invention is not limited to following given example.
The side's of enforcement example 1: the preparation method of tri compound photochemical catalyst of the present invention comprises the following steps:
(1) prepare BiPO
4: the 2mmol bismuth nitrate is dissolved in the salpeter solution that concentration is 2mol/L, forms clear solution, under stirring, slowly add 0.1mol/L citric acid solution 20mL, continue to stir 0.5h, then add the sodium radio-phosphate,P-32 solution that measures ratio, wherein the concentration of sodium phosphate is controlled at 0.1mol/L, stir 0.5h, then proceed to 50mL containing in teflon-lined stainless steel autoclave, 180 ℃ of reaction 24h, by the products therefrom centrifugation, and, 60 ℃ of vacuum drying, obtain BiPO
4photochemical catalyst;
(2) preparation of tri compound photochemical catalyst: get BiPO prepared by step (1)
4photochemical catalyst 0.5g adds ultrasonic dispersion in the hydrochloric acid solution of 50mL0.5mol/L, add the 0.025g aniline monomer under room temperature, logical nitrogen is after 40 minutes, add the 0.065g ammonium persulfate, room temperature reaction 4h, carry out suction filtration by product, after water and absolute ethyl alcohol wash respectively for several times, dry in 50 ℃ of vacuum drying ovens, obtain polyaniline, BiOCl, BiPO
4the tri compound photochemical catalyst.
As shown in Figure 1, the phase of tri compound photochemical catalyst being characterized, is Tetragonal BiOCl (JCPDS85-0861) but the diffraction maximum that triangle sections out is index, but the BiPO that remaining diffraction maximum index is monoclinic phase
4(JCPDS89-0287), the characteristic peak of polyaniline do not find, may be lower with its content and crystallinity is poor relevant, and this result tentatively illustrates that the existence of hydrochloric acid has etched away part BiPO
4, formed BiOCl.Pattern through SEM to the tri compound photochemical catalyst characterizes, and wherein bulk morphologies is BiPO
4photochemical catalyst, bar-shaped area load a lot of granules be polyaniline, illustrate that polyaniline is at BiPO
4the surface aggregate success, also have a small amount of sheet BiOCl to form, as shown in Figure 2 in addition.Utilize Fourier infrared spectrograph to carry out structural characterization to product, as shown in Figure 3, as can be seen from the figure the tri compound photochemical catalyst is by polyaniline, BiOCl, BiPO
4form, illustrate that composite photo-catalyst is successfully prepared.Tri compound photochemical catalyst and BiPO
4photocatalysis performance be that degradation of methylene blue under the radiation of visible light provided by the 500W xenon lamp (methylene blue, MB) solution is weighed, concrete experimentation is as follows: taking the 100mg photochemical catalyst, to add concentration be 10
-5in the 100mL MB solution of M, the solution prepared is placed in to the dark place dispersed with stirring and within 2 hours, makes it reach adsorption equilibrium.Then solution is carried out to light-catalyzed reaction, get at regular intervals the solution of about 5mL, catalyst is fallen in centrifugal filtration, with ultraviolet specrophotometer, measures MB absorbance residual in solution.Tri compound photochemical catalyst and BiPO
4photocatalysis performance as shown in Figure 4, its result shows that tri compound photochemical catalyst photocatalysis performance obviously is better than pure BiPO
4photocatalysis performance under visible ray.
Embodiment 2: the preparation method of a kind of tri compound photochemical catalyst of the present invention comprises the following steps:
(1) prepare BiPO
4: the 2mmol bismuth nitrate is dissolved in the salpeter solution that concentration is 1mol/L, forms clear solution, under stirring, slowly add 0.2mol/L citric acid solution 10mL, continue to stir 0.5h, then add the dibastic sodium phosphate solution that measures ratio, wherein the concentration of dibastic sodium phosphate is controlled at 0.2mol/L, stir 0.5h, then proceed to 50mL containing in teflon-lined stainless steel autoclave, 190 ℃ of reaction 20h, by the products therefrom centrifugation, and, 60 ℃ of vacuum drying, obtain BiPO
4photochemical catalyst;
(2) preparation of tri compound photochemical catalyst: get BiPO prepared by step (1)
4photochemical catalyst 0.5g adds ultrasonic dispersion in the hydrochloric acid solution of 50mL0.4mol/L, add the 0.05g aniline monomer under room temperature, logical nitrogen is after 30 minutes, add the 0.13g ammonium persulfate, room temperature reaction 6h, carry out suction filtration by product, after water and absolute ethyl alcohol wash respectively for several times, dry in 60 ℃ of vacuum drying ovens, obtain polyaniline, BiOCl, BiPO
4the tri compound photochemical catalyst.
Embodiment 3: a kind of conducting polymer/BiPO of the present invention
4the preparation method of composite photo-catalyst, comprise the steps:
(1) prepare BiPO
4: the 2mmol bismuth nitrate is dissolved in the salpeter solution that concentration is 1mol/L, forms clear solution, under stirring, slowly add 0.1mol/L citric acid solution 20mL, continue to stir 0.5h, then add the dibastic sodium phosphate solution that measures ratio, wherein the concentration of sodium dihydrogen phosphate is controlled at 0.1mol/L, stir 0.5h, then proceed to 50mL containing in teflon-lined stainless steel autoclave, 200 ℃ of reaction 15h, by the products therefrom centrifugation, and, 50 ℃ of vacuum drying, obtain BiPO
4photochemical catalyst;
(2) preparation of tri compound photochemical catalyst: get BiPO prepared by step (1)
4photochemical catalyst 0.5g adds ultrasonic dispersion in the hydrochloric acid solution of 50mL0.4mol/L, add the 0.04g aniline monomer under room temperature, logical nitrogen is after 30 minutes, add the 0.1g ammonium persulfate, room temperature reaction 6h, carry out suction filtration by product, after water and absolute ethyl alcohol wash respectively for several times, dry in 60 ℃ of vacuum drying ovens, obtain polyaniline, BiOCl, BiPO
4the tri compound photochemical catalyst.
Claims (3)
1. tri compound photochemical catalyst and preparation method thereof, is characterized in that: by three component polyanilines, BiOCl, BiPO
4be composited, utilize polyaniline, BiOCl to BiPO
4synergy, widened BiPO
4spectral response range, be beneficial to the separation in light induced electron-hole, make composite photo-catalyst there is the visible light catalytic performance, comprise the steps:
(1) prepare BiPO
4: a certain amount of bismuth salt is dissolved in the salpeter solution that concentration is 0.1～5mol/L, form clear solution, under stirring, slowly add 0.1～0.5mol/L citric acid solution, 5～20mL, continue to stir 0.5～1h, add again the phosphate solution that measures ratio, wherein phosphatic concentration is controlled at 0.01～0.1mol/L, stir 0.5～1h, then proceed to 50mL containing in teflon-lined stainless steel autoclave, 100～240 ℃ of reaction 10～30h, by the products therefrom centrifugation, and, 50～100 ℃ of vacuum drying, obtain BiPO
4photochemical catalyst:
(2) preparation of tri compound photochemical catalyst: get BiPO prepared by step (1)
4photochemical catalyst 0.1～0.5g adds ultrasonic dispersion in the certain density hydrochloric acid solution of 50mL, add aniline monomer under room temperature, logical nitrogen is after 20～60 minutes, add a certain amount of ammonium persulfate, room temperature reaction 0.5～10h, product is carried out to suction filtration, after water and absolute ethyl alcohol wash respectively for several times, dry in 60 ℃ of vacuum drying ovens.
2. the preparation method of tri compound photochemical catalyst according to claim 1, is characterized in that bismuth salt in step (1) is a kind of in bismuth nitrate, bismuth chloride, and phosphate is a kind of in sodium phosphate, dibastic sodium phosphate, sodium dihydrogen phosphate.
3. the preparation method of tri compound photochemical catalyst according to claim 1, is characterized in that in step (2), concentration of hydrochloric acid is 0.1～0.5mo1/L, aniline and BiPO
4mass ratio be 1:100～10:100, the amount of substance of aniline and the amount of substance of ammonium persulfate are 1: 1～1:3.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108380241A (en) * | 2018-03-27 | 2018-08-10 | 昆明理工大学 | A kind of Z-type photochemical catalyst BiPO4The preparation and its application of/H-ZSM-5/BiOCl |
| CN108855194A (en) * | 2018-07-27 | 2018-11-23 | 章立兰 | A kind of nitrogen-doped nanometer BiOX type photochemical catalyst of high catalytic activity and preparation method thereof |
| CN108940332A (en) * | 2018-06-04 | 2018-12-07 | 东北大学 | A kind of high activity MoS2/g-C3N4/Bi24O31Cl10The preparation method of composite photo-catalyst |
| CN110075883A (en) * | 2019-05-30 | 2019-08-02 | 江汉大学 | A kind of BiPO4The preparation method of nano-photocatalyst |
| CN110252416A (en) * | 2019-06-12 | 2019-09-20 | 盐城工学院 | A kind of bismuth oxybromide@polyaniline-manganese dioxide composite photo-catalyst and its preparation method and application |
| CN111398385A (en) * | 2020-05-10 | 2020-07-10 | 陈先丽 | Composite electrode for heavy metal ion detection and preparation method thereof |
| CN113546648A (en) * | 2021-07-28 | 2021-10-26 | 西北师范大学 | Preparation method of ultrathin nano wafer-shaped BiOBr high-activity photocatalyst |
| CN114950509A (en) * | 2022-05-31 | 2022-08-30 | 齐齐哈尔大学 | Catalyst for microwave activation persulfate rapid oxidative degradation of PPCPs wastewater and preparation and application methods thereof |
| CN115155629A (en) * | 2022-06-29 | 2022-10-11 | 衢州学院 | Bi/BiPO 4 Preparation method and application of/BiOCl nanosheet composite material |
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Cited By (16)
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| CN108380241B (en) * | 2018-03-27 | 2020-12-22 | 昆明理工大学 | Z-type photocatalyst BiPO4Preparation and application of/H-ZSM-5/BiOCl |
| CN108380241A (en) * | 2018-03-27 | 2018-08-10 | 昆明理工大学 | A kind of Z-type photochemical catalyst BiPO4The preparation and its application of/H-ZSM-5/BiOCl |
| CN108940332A (en) * | 2018-06-04 | 2018-12-07 | 东北大学 | A kind of high activity MoS2/g-C3N4/Bi24O31Cl10The preparation method of composite photo-catalyst |
| CN108940332B (en) * | 2018-06-04 | 2020-12-15 | 东北大学 | High-activity MoS2/g-C3N4/Bi24O31Cl10Preparation method of composite photocatalyst |
| CN108855194A (en) * | 2018-07-27 | 2018-11-23 | 章立兰 | A kind of nitrogen-doped nanometer BiOX type photochemical catalyst of high catalytic activity and preparation method thereof |
| CN108855194B (en) * | 2018-07-27 | 2021-07-16 | 章立兰 | Nitrogen-doped nano BiOX type photocatalyst with high catalytic activity and preparation method thereof |
| CN110075883A (en) * | 2019-05-30 | 2019-08-02 | 江汉大学 | A kind of BiPO4The preparation method of nano-photocatalyst |
| CN110252416A (en) * | 2019-06-12 | 2019-09-20 | 盐城工学院 | A kind of bismuth oxybromide@polyaniline-manganese dioxide composite photo-catalyst and its preparation method and application |
| CN111398385A (en) * | 2020-05-10 | 2020-07-10 | 陈先丽 | Composite electrode for heavy metal ion detection and preparation method thereof |
| CN111398385B (en) * | 2020-05-10 | 2023-12-29 | 北京怀胜高科技产业发展有限公司 | Composite electrode for heavy metal ion detection and preparation method thereof |
| CN113546648A (en) * | 2021-07-28 | 2021-10-26 | 西北师范大学 | Preparation method of ultrathin nano wafer-shaped BiOBr high-activity photocatalyst |
| CN113546648B (en) * | 2021-07-28 | 2022-04-19 | 西北师范大学 | Preparation method of ultrathin nano wafer-shaped BiOBr high-activity photocatalyst |
| CN114950509A (en) * | 2022-05-31 | 2022-08-30 | 齐齐哈尔大学 | Catalyst for microwave activation persulfate rapid oxidative degradation of PPCPs wastewater and preparation and application methods thereof |
| CN114950509B (en) * | 2022-05-31 | 2023-06-20 | 齐齐哈尔大学 | Microwave activated persulfate rapid oxidative degradation PPCPs wastewater catalyst and preparation and application methods thereof |
| CN115155629A (en) * | 2022-06-29 | 2022-10-11 | 衢州学院 | Bi/BiPO 4 Preparation method and application of/BiOCl nanosheet composite material |
| CN115155629B (en) * | 2022-06-29 | 2023-05-02 | 衢州学院 | Bi/BiPO 4 Preparation method and application of BiOCl nano-sheet composite material |
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