CN106984360A - Bi2O2CO3/PPy/g‑C3N4Composite photo-catalyst and its preparation method and application - Google Patents
Bi2O2CO3/PPy/g‑C3N4Composite photo-catalyst and its preparation method and application Download PDFInfo
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 58
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 229920000128 polypyrrole Polymers 0.000 claims abstract description 81
- 239000002131 composite material Substances 0.000 claims abstract description 65
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229940043267 rhodamine b Drugs 0.000 claims abstract description 18
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 13
- 239000010439 graphite Substances 0.000 claims abstract description 13
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 claims abstract description 13
- 230000001699 photocatalysis Effects 0.000 claims abstract description 10
- 238000007146 photocatalysis Methods 0.000 claims abstract description 10
- 239000000975 dye Substances 0.000 claims abstract description 9
- 229910000014 Bismuth subcarbonate Inorganic materials 0.000 claims abstract description 8
- MGLUJXPJRXTKJM-UHFFFAOYSA-L bismuth subcarbonate Chemical compound O=[Bi]OC(=O)O[Bi]=O MGLUJXPJRXTKJM-UHFFFAOYSA-L 0.000 claims abstract description 8
- 229940036358 bismuth subcarbonate Drugs 0.000 claims abstract description 8
- 239000000463 material Substances 0.000 claims abstract description 8
- 239000002351 wastewater Substances 0.000 claims abstract description 5
- 238000006555 catalytic reaction Methods 0.000 claims abstract description 4
- 239000000203 mixture Substances 0.000 claims abstract description 3
- 238000006243 chemical reaction Methods 0.000 claims description 35
- 238000000034 method Methods 0.000 claims description 23
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- 239000003054 catalyst Substances 0.000 claims description 18
- 239000003495 polar organic solvent Substances 0.000 claims description 14
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 239000004677 Nylon Substances 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 9
- 239000012528 membrane Substances 0.000 claims description 9
- 229920001778 nylon Polymers 0.000 claims description 9
- 239000000843 powder Substances 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 8
- 238000002604 ultrasonography Methods 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 3
- 239000000376 reactant Substances 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical group OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 claims description 2
- 238000011282 treatment Methods 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 11
- 230000004044 response Effects 0.000 abstract description 9
- 230000015556 catabolic process Effects 0.000 abstract description 7
- 238000006731 degradation reaction Methods 0.000 abstract description 7
- 230000008901 benefit Effects 0.000 abstract description 2
- 230000000593 degrading effect Effects 0.000 abstract description 2
- 238000012545 processing Methods 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 239000003344 environmental pollutant Substances 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- 239000003960 organic solvent Substances 0.000 abstract 1
- 231100000719 pollutant Toxicity 0.000 abstract 1
- 238000010992 reflux Methods 0.000 abstract 1
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- 238000010189 synthetic method Methods 0.000 abstract 1
- 238000001291 vacuum drying Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 13
- 238000010586 diagram Methods 0.000 description 12
- 239000007864 aqueous solution Substances 0.000 description 6
- 239000004065 semiconductor Substances 0.000 description 6
- 230000003197 catalytic effect Effects 0.000 description 5
- 238000001069 Raman spectroscopy Methods 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 150000001621 bismuth Chemical class 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052736 halogen Inorganic materials 0.000 description 2
- 150000002367 halogens Chemical class 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000009738 saturating Methods 0.000 description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- 239000010937 tungsten Substances 0.000 description 2
- 238000002371 ultraviolet--visible spectrum Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- CKUAXEQHGKSLHN-UHFFFAOYSA-N [C].[N] Chemical compound [C].[N] CKUAXEQHGKSLHN-UHFFFAOYSA-N 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000002322 conducting polymer Substances 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- 230000002079 cooperative effect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000010919 dye waste Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/06—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing polymers
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
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- Health & Medical Sciences (AREA)
- Toxicology (AREA)
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Abstract
The invention belongs to the catalysis material technical field of degrading waste water pollutant, Bi is disclosed2O2CO3/PPy/g‑C3N4Composite photo-catalyst preparation and its under simulated solar irradiation rhodamine B degradation application.Synthesis step includes：Bismuth subcarbonate (the Bi that polypyrrole PPy is adulterated2O2CO3) composite and graphite phase carbon nitride (g C3N4) mix in proportion in organic solvent, it is heated to reflux, products therefrom is washed for several times, and Bi is produced after vacuum drying2O2CO3/PPy/g‑C3N4Photocatalysis composite.The advantage of the invention is that synthetic method is simple, it is easy to large-scale industrial production, prepared composite properties are stable, photocatalytic activity is high, expanded Bi2O2CO3Spectral response range, improve the utilization rate to sunshine, there is preferable degradation effect to certain density organic dyestuff rhodamine B, the processing of waste water from dyestuff is can be applied to.
Description
Technical field
The invention belongs to photochemical catalyst field, and in particular to a series of ternary systems with simulated solar photolytic activity
Bi2O2CO3/PPy/g-C3N4The preparation and its application of composite photo-catalyst.
Background technology
As developing rapidly for industry is increasing with population, environmental pollution and the shortage of critical energy have become system
About two hang-ups of human social development.Solar energy is a kind of abundant, cleaning sustainable energy, and photocatalysis is recycling
The effective means of solar energy.Photocatalysis technology can be using abundant solar energy come degradable organic pollutant etc., and this is to solving ring
Border crisis has very important meaning, wherein the significantly application of Photocatalitic Technique of Semiconductor.However, current light is urged
There are two shortcomings in agent：(1) utilization rate to sunshine is not high；(2) light induced electron is easily combined with hole.Research has shown that,
Composite semiconductor material is the effective way for solving above-mentioned two problems.
Bismuth series photocatalyst (such as bismuth subcarbonate) have good catalytic performance and excellent chemical stability, in recent years by
It is widely studied.They have obvious absorption in visible-range, and this is the common distinguishing feature and advantage of bismuth series photocatalyst,
And they have good catalytic action to hardly degraded organic substance under visible light, it is possible to recycle, be applied to work
Industry sewage disposal by be future studies a hot fields.Graphite phase carbon nitride g-C3N4It is that one kind is made up of non-metal carbon nitrogen
Visible-light photocatalyst, it is similar with graphene, with two-dimension plane structure；There is typical characteristic of semiconductor simultaneously, it is prohibited
Bandwidth is about 2.7eV, can ultraviolet-visible light of the absorbing wavelength less than 470nm.Because of its unique structure, g-C3N4Base complex light
Catalyst shows good photocatalysis performance.Polypyrrole has excellent electric conductivity, narrow energy gap, good environment
Stability and formability, by the change of substituent, performance can be with modulation, and compared with other conducting polymers, can be in water
In prepared by chemical oxidative polymerization.But pair and polypyrrole, particularly and polypyrrole and g-C3N4 codopes are answered
The photochemical catalyst research of conjunction is relatively fewer.Answering for photo-generated carrier can effectively be suppressed by building the composite semiconductor of heterojunction structure
Close, be a kind of efficient semiconductor method of modifying so as to improve the photocatalytic activity of semiconductor.
Therefore, we attempt to design, are prepared for a series of Bi2O2CO3/PPy/g-C3N4Composite photo-catalyst, expands light and urges
Agent inquires into g-C to the response range of visible ray3N4Influence of the content to composite photo-catalyst catalytic performance.It is so far
Only, Bi is prepared2O2CO3/PPy/g-C3N4There is not been reported for the work of composite photo-catalyst, also without patent and document report mistake
Bi2O2CO3/PPy/g-C3N4The preparation of composite photo-catalyst and Study on Performance.
The content of the invention
It is an object of the invention to provide a kind of ternary system Bi with simulated solar photolytic activity2O2CO3/PPy/g-C3N4
The preparation method of composite photo-catalyst, to improve catalysis material to visible ray and the spectrum utilization factor of near infrared region, it is made
Standby technique is simple, easily realizes, the composite photo-catalyst of preparation has good sun photolytic activity and higher quantum efficiency, right
Organic dye waste water has preferable degradation effect, has weight in fields such as the purified treatments and organic waste-gas purification of organic wastewater
Want application prospect.
In order to solve the above technical problems, the present invention uses following technical scheme：
Bi of the present invention2O2CO3/PPy/g-C3N4Composite photo-catalyst, compares Bi by secondary carbonic acid2O2CO3, polypyrrole PPy
With graphite phase carbon nitride g-C3N4Composition, the composite photocatalyst material is under simulated solar light irradiation after 90min, and rhodamine B drops
Solution rate is 98.94%.
Bi of the present invention2O2CO3/PPy/g-C3N4The preparation method of composite photo-catalyst, comprises the following steps：
Step A1：By bismuth subcarbonate Bi2O2CO3It is organic molten in polarity by certain quality ratio ultrasonic disperse with polypyrrole PPy
In agent, after being uniformly dispersed, back flow reaction is carried out；After reaction terminates, by reactant through cooling down, filtering, wash, dry, ash is obtained
Color powdery product, as Bi2O2CO3/ PPy composite photo-catalysts；
Step A2：First by step A1 products therefroms Bi2O2CO3/ PPy ultrasonic disperses are in polar organic solvent, under ultrasound,
Add a certain amount of graphite phase carbon nitride g-C3N4, continue ultrasound, after being uniformly dispersed, carry out back flow reaction；After reaction terminates,
By reactant through cooling, filtering, washing, dry, obtain grey powder product, as Bi2O2CO3/PPy/g-C3N4Complex light
Catalyst.
Step A1 and A2 polar organic solvent are tetrahydrofuran.
In step A1, the bismuth subcarbonate Bi2O2CO3Mass ratio with polypyrrole PPy is 100:1；
In step A2, the Bi2O2CO3/ PPy composite photo-catalysts and graphite phase carbon nitride g-C3N4Mass ratio be
1000:1~1000:20；
In step A1, the ultrasonic time is 2 hours, and back flow reaction temperature is 66 DEG C, and the reaction time is 24 hours；
In step A2, the ultrasound is first by Bi2O2CO3/ PPy ultrasound 1 hour in polar organic solvent tetrahydrofuran,
Then g-C is added3N4Ultrasonic 1 hour again, the temperature of back flow reaction is 66 DEG C, and the reaction time is 12 hours.
Separation is to be filtered reaction solution with 0.45 μm of nylon membrane described in the preparation method；The washing is
Washed respectively with deionized water and ethanol；The drying is that vacuum is dried 12 hours at room temperature.
The composite photo-catalyst, works as Bi2O2CO3/ PPy composite photo-catalysts and graphite phase carbon nitride g-C3N4Mass ratio
For 1000：When 5, the catalytic effect of material is optimal；The clearance of rhodamine B is up to 98.94%.
Application process described in the composite photo-catalyst is：By Bi2O2CO3/PPy/g-C3N4Composite photo-catalyst and dyestuff
Rhodamine B is mixed to get mixed liquor under light protected environment, and the mixed liquor is carried out into light-catalyzed reaction 15- under simulated solar irradiation
90min, completes the processing to dye, rhodamine B.
Relative to prior art, beneficial effects of the present invention are：
(1) Bi that the present invention is prepared using hydro-thermal method2O2CO3/PPy/g-C3N4Composite photocatalyst, with equal bar
The Bi prepared under part2O2CO3/ PPy composites and pure Bi2O2CO3Compare, ternary system Bi2O2CO3/PPy/g-C3N4Complex light
Catalyst shows higher photocatalytic activity and simulated solar light utilization efficiency.
(2) the ternary system Bi2O2CO3/PPy/g-C3N4In composite photo-catalyst, Bi2O2CO3, PPy and g-C3N4Three
Cooperative effect between person, promotes the separative efficiency of photo-generated carrier, effectively inhibits the compound of photo-generated carrier, improves
The catalytic activity of composite photo-catalyst.
(3) the ternary system Bi2O2CO3/PPy/g-C3N4Composite photo-catalyst photo-thermal is stablized, and activity is high, can be multiple
Reuse；PPy and g-C3N4Introducing reduce Bi2O2CO3Energy gap so that improve its mould to intend sunshine sound
Scope is answered, there is good degradation effect to organic pollution rhodamine B.
Brief description of the drawings
Fig. 1 is ternary system Bi prepared by the inventive method2O2CO3/PPy/g-C3N4Composite photo-catalyst is not sensitized with BP,
Bi2O2CO3The infrared comparison diagram of photochemical catalyst；
Fig. 2 is ternary system BP/C0.5, BP prepared by the inventive method and the Bi not being sensitized2O2CO3The XRD of photochemical catalyst
Comparison diagram；
Fig. 3 is ternary system BP/C0.5, BP prepared by the inventive method and the Bi not being sensitized2O2CO3Photochemical catalyst
Raman comparison diagrams；
Fig. 4 is ternary system BP/C0.5, BP prepared by the inventive method and the Bi not being sensitized2O2CO3Photochemical catalyst it is saturating
Penetrate electron microscope, a-Bi2O2CO3, b-BP and c-BP/C0.5；
Fig. 5 is ternary system BP/C0.5, BP, g-C prepared by the inventive method3N4The Bi not being sensitized2O2CO3Photocatalysis
The UV-Vis DRS spectrum comparison diagram of agent；
Fig. 6 is ternary system BP/C0.5, BP prepared by the inventive method and the Bi not being sensitized2O2CO3The light of photochemical catalyst
Current-responsive comparison diagram；
Fig. 7 is ternary system BP/C0.5, BP prepared by the inventive method and the Bi not being sensitized2O2CO3The resistance of photochemical catalyst
Anti- comparison diagram；
Fig. 8 is ternary system Bi prepared by the inventive method2O2CO3/PPy/g-C3N4Composite photo-catalyst is not sensitized with BP,
Bi2O2CO3And g-C3N4Photocatalyst for degrading rhodamine B aqueous solution degradation rate time history plot；
Fig. 9 be the inventive method prepare the ternary system composite photo-catalyst BP/C0.5 rhodamine B degradations aqueous solution at any time
Between the UV-visible spectrum that changes.
Embodiment
Below by way of specific embodiment, present invention is described or is further described, and gives detailed reality
Mode and specific operating process are applied, its object is to more fully understand the technical connotation of the present invention, but the protection model of the present invention
Enclose and be not limited to following embodiments.
Embodiment 1：
By bismuth subcarbonate Bi2O2CO3(200mg) and polypyrrole PPy (2mg) ultrasonic disperse (2 hours) is in polar organic solvent
In tetrahydrofuran (20mL), back flow reaction is carried out after being uniformly dispersed, at 66 DEG C 24 hours.After reaction terminates, the cooling of question response liquid
To room temperature, reaction solution is filtered with 0.45 μm of nylon membrane, then washed respectively with deionized water and ethanol, then in room
Drying obtains grey powder product, as Bi in 12 hours under warm vacuum2O2CO3/ PPy (BP) composite photo-catalyst.
Wherein, bismuth subcarbonate Bi2O2CO3Mass ratio with polypyrrole PPy is 100:1.
Embodiment 2：
BP composites (80mg) ultrasonic disperse prepared by embodiment 1 is at polar organic solvent tetrahydrofuran (20mL)
In, ultrasonic time is 1 hour.Then g-C is added3N4(0.08mg) is ultrasonic 1 hour again, after being uniformly dispersed, is flowed back at 66 DEG C
Reaction 12 hours.After reaction terminates, question response liquid is cooled to after room temperature, and reaction solution is filtered with 0.45 μm of nylon membrane,
Washed respectively with deionized water and ethanol again, then drying obtains grey powder product in 12 hours under room temperature in vacuo, be
BP/C0.1 composite photo-catalysts.
Wherein, BP and g-C3N4Mass ratio be 1000:1.
Embodiment 3：
BP composites (80mg) ultrasonic disperse prepared by embodiment 1 is at polar organic solvent tetrahydrofuran (20mL)
In, ultrasonic time is 1 hour.Then g-C is added3N4(0.2mg) is ultrasonic 1 hour again, after being uniformly dispersed, is flowed back at 66 DEG C
Reaction 12 hours.After reaction terminates, question response liquid is cooled to after room temperature, and reaction solution is filtered with 0.45 μm of nylon membrane,
Washed respectively with deionized water and ethanol again, then drying obtains grey powder product in 12 hours under room temperature in vacuo, be
BP/C0.25 composite photo-catalysts.
Wherein, BP and g-C3N4Mass ratio be 1000:2.5.
Embodiment 4：
BP composites (80mg) ultrasonic disperse prepared by embodiment 1 is at polar organic solvent tetrahydrofuran (20mL)
In, ultrasonic time is 1 hour.Then g-C is added3N4(0.4mg) is ultrasonic 1 hour again, after being uniformly dispersed, is flowed back at 66 DEG C
Reaction 12 hours.After reaction terminates, question response liquid is cooled to after room temperature, and reaction solution is filtered with 0.45 μm of nylon membrane,
Washed respectively with deionized water and ethanol again, then drying obtains grey powder product in 12 hours under room temperature in vacuo, be
BP/C0.5 composite photo-catalysts.
Wherein, BP and g-C3N4Mass ratio be 1000:5.
Embodiment 5：
BP composites (80mg) ultrasonic disperse prepared by embodiment 1 is at polar organic solvent tetrahydrofuran (20mL)
In, ultrasonic time is 1 hour.Then g-C is added3N4(0.8mg) is ultrasonic 1 hour again, after being uniformly dispersed, is flowed back at 66 DEG C
Reaction 12 hours.After reaction terminates, question response liquid is cooled to after room temperature, and reaction solution is filtered with 0.45 μm of nylon membrane,
Washed respectively with deionized water and ethanol again, then drying obtains grey powder product in 12 hours under room temperature in vacuo, be
BP/C1.0 composite photo-catalysts.
Wherein, BP and g-C3N4Mass ratio be 1000:10.
Embodiment 6：
BP composites (80mg) ultrasonic disperse prepared by embodiment 1 is at polar organic solvent tetrahydrofuran (20mL)
In, ultrasonic time is 1 hour.Then g-C is added3N4(1.2mg) is ultrasonic 1 hour again, after being uniformly dispersed, is flowed back at 66 DEG C
Reaction 12 hours.After reaction terminates, question response liquid is cooled to after room temperature, and reaction solution is filtered with 0.45 μm of nylon membrane,
Washed respectively with deionized water and ethanol again, then drying obtains grey powder product in 12 hours under room temperature in vacuo, be
BP/C1.5 composite photo-catalysts.
Wherein, BP and g-C3N4Mass ratio be 1000:15.
Embodiment 7：
BP composites (80mg) ultrasonic disperse prepared by embodiment 1 is at polar organic solvent tetrahydrofuran (20mL)
In, ultrasonic time is 1 hour.Then g-C is added3N4(1.6mg) is ultrasonic 1 hour again, after being uniformly dispersed, is flowed back at 66 DEG C
Reaction 12 hours.After reaction terminates, question response liquid is cooled to after room temperature, and reaction solution is filtered with 0.45 μm of nylon membrane,
Washed respectively with deionized water and ethanol again, then drying obtains grey powder product in 12 hours under room temperature in vacuo, be
BP/C2.0 composite photo-catalysts.
Wherein, BP and g-C3N4Mass ratio be 1000:20.
Fig. 1 is ternary system Bi prepared by the inventive method2O2CO3/PPy/g-C3N4Composite photo-catalyst is not sensitized with BP,
Bi2O2CO3The infrared comparison diagram of photochemical catalyst；The infrared spectrum shows polypyrrole PPy and graphite phase carbon nitride g-C3N4Draw
Enter.
Fig. 2 is ternary system BP/C0.5, BP prepared by the inventive method and the Bi not being sensitized2O2CO3The XRD of photochemical catalyst
Comparison diagram；The XRD spectra also indicates that polypyrrole PPy and graphite phase carbon nitride g-C3N4Introducing.
Fig. 3 is ternary system BP/C0.5, BP prepared by the inventive method and the Bi not being sensitized2O2CO3Photochemical catalyst
Raman comparison diagrams；The Raman spectrograms show polypyrrole PPy and graphite phase carbon nitride g-C3N4Introducing.
Fig. 4 is ternary system BP/C0.5, BP prepared by the inventive method and the Bi not being sensitized2O2CO3Photochemical catalyst it is saturating
Penetrate electron microscope, a-Bi2O2CO3, b-BP and c-BP/C0.5；Wherein, figure b and c shows polypyrrole PPy and graphite-phase compared with scheming a
Carbonitride g-C3N4Introducing.
Fig. 5 is ternary system BP/C0.5, BP, g-C prepared by the inventive method3N4The Bi not being sensitized2O2CO3Photocatalysis
The UV-Vis DRS spectrum comparison diagram of agent；The UV-Vis DRS spectrogram shows polypyrrole PPy and graphite-phase nitrogen
Change carbon g-C3N4Introducing, and the introducing of the two extends Bi2O2CO3In the absorption of visible region.
Fig. 6 is ternary system BP/C0.5, BP prepared by the inventive method and the Bi not being sensitized2O2CO3The light of photochemical catalyst
Current-responsive comparison diagram；The spectrogram shows Bi2O2CO3, PPy and g-C3N4Cooperative effect between three, promotes photoproduction current-carrying
The separative efficiency of son, effectively inhibits the compound of photo-generated carrier.
Fig. 7 is ternary system BP/C0.5, BP prepared by the inventive method and the Bi not being sensitized2O2CO3The resistance of photochemical catalyst
Anti- comparison diagram；The spectrogram shows PPy and g-C3N4Introducing reduce Bi2O2CO3Resistance, improve its electric conductivity, be conducive to
The separation of photo-generated carrier and being combined for suppression photo-generated carrier.
Comparative example is below by comparative example to a series of Bi for being prepared in the present invention2O2CO3/PPy/g-C3N4Composite photocatalyst
Agent illustrates the effect of composite photocatalyst material under simulated solar irradiation to the degraded percentage of the rhodamine B aqueous solution.
In order to verify a series of Bi prepared by the present invention2O2CO3/PPy/g-C3N4The potential application of composite photo-catalyst,
Inventor is by itself and Bi2O2CO3、g-C3N4With BP under same light source radiation, a series of contrasts are done.Using the rhodamine B aqueous solution as
Target solution, the light source that photocatalysis experiment is used is 350W halogen tungsten lamp.Target solution is placed in 100mL beakers, and beaker hangs down with lamp
Straight to place, distance therebetween is 15 centimetres.Calculated and dropped according to the change of rhodamine B aqueous solution absorbance before and after illumination
Percentage is solved, comparing result is as shown in Figure 8.
Fig. 8 is the Bi not being sensitized with 50mg2O2CO3、g-C3N4, BP and Bi2O2CO3/PPy/g-C3N4Composite photo-catalyst drops
Solve the 50mL10mg/L rhodamine Bs solution curve that solution absorptance is changed over time under light source.As can be seen from Figure 8, exist
Under the conditions of 350W halogen tungsten light irradiations, the ternary system composite photo-catalyst BP/C0.5 prepared by the present invention has than not being sensitized
Bi2O2CO3、g-C3N4With the more preferable photocatalysis effects of BP.Show Bi2O2CO3, PPy and g-C3N4Cooperative effect between three,
The separative efficiency of photo-generated carrier is promoted, the compound of photo-generated carrier is restrained effectively, so as to improve Bi2O2CO3In mould
Intend the photocatalysis effect under sunshine.
Fig. 9 be the inventive method prepare the ternary system composite photo-catalyst BP/C0.5 rhodamine B degradations aqueous solution at any time
Between the UV-visible spectrum that changes；The spectrogram shows that rhodamine B is progressively decomposed under light illumination, and almost complete after 90 minutes
Degrade in portion.
Claims (8)
1.Bi2O2CO3/PPy/g-C3N4Composite photo-catalyst, it is characterised in that Bi is compared by secondary carbonic acid2O2CO3, polypyrrole PPy and
Graphite phase carbon nitride g-C3N4Composition, the composite photocatalyst material is under simulated solar light irradiation after 90min, and rhodamine B is degraded
Rate is 98.94%.
2. Bi according to claim 12O2CO3/PPy/g-C3N4The preparation method of composite photo-catalyst, it is characterised in that
Comprise the following steps：
Step A1：By bismuth subcarbonate Bi2O2CO3With polypyrrole PPy by certain quality ratio ultrasonic disperse in polar organic solvent
In, after being uniformly dispersed, carry out back flow reaction；After reaction terminates, by reactant through cooling, filtering, washing, dry, obtain grey
Powdery product, as Bi2O2CO3/ PPy composite photo-catalysts；
Step A2：First by step A1 products therefroms Bi2O2CO3/ PPy ultrasonic disperses are in polar organic solvent, under ultrasound, then add
Enter a certain amount of graphite phase carbon nitride g-C3N4, continue ultrasound, after being uniformly dispersed, carry out back flow reaction；, will be anti-after reaction terminates
Answer thing through cooling, filtering, washing, dry, obtain grey powder product, as Bi2O2CO3/PPy/g-C3N4Composite photocatalyst
Agent.
3. Bi according to claim 22O2CO3/PPy/g-C3N4The preparation method of composite photo-catalyst, it is characterised in that
In the preparation method, step A1 and A2 polar organic solvent are tetrahydrofuran.
In step A1, the bismuth subcarbonate Bi2O2CO3Mass ratio with polypyrrole PPy is 100:1；
In step A2, the Bi2O2CO3/ PPy composite photo-catalysts and graphite phase carbon nitride g-C3N4Mass ratio be 1000:1~
1000:20。
4. Bi according to claim 32O2CO3/PPy/g-C3N4The preparation method of composite photo-catalyst, it is characterised in that
Work as Bi2O2CO3/ PPy composite photo-catalysts and graphite phase carbon nitride g-C3N4Mass ratio be 1000：5.
5. Bi according to claim 22O2CO3/PPy/g-C3N4The preparation method of composite photo-catalyst, it is characterised in that
In the preparation method, step A1 ultrasonic time is 2 hours, and the temperature of back flow reaction is 66 DEG C, and the reaction time is 24 hours；
Ultrasound in step A2 is first by Bi2O2CO3/ PPy ultrasound 1 hour in polar organic solvent tetrahydrofuran, then adds g-
C3N4Ultrasonic 1 hour again, back flow reaction temperature is 66 DEG C, and the reaction time is 12 hours.
6. Bi according to claim 22O2CO3/PPy/g-C3N4The preparation method of composite photo-catalyst, it is characterised in that
In the preparation method, the separation is to be filtered reaction solution with 0.45 μm of nylon membrane；The washing is to use respectively
Deionized water and ethanol washing；The drying is that vacuum is dried 12 hours at room temperature.
7. Bi according to claim 12O2CO3/PPy/g-C3N4The purposes of composite photo-catalyst, it is characterised in that by institute
The Bi stated2O2CO3/PPy/g-C3N4Composite catalyst as photocatalysis treatment waste water from dyestuff green material；The dyestuff
Dyestuff in waste water is rhodamine B.
8. Bi according to claim 72O2CO3/PPy/g-C3N4The purposes of composite photo-catalyst, it is characterised in that described
Application process is：By Bi2O2CO3/PPy/g-C3N4Composite photo-catalyst and dye, rhodamine B are mixed to get mixed under light protected environment
Liquid is closed, the mixed liquor is subjected to light-catalyzed reaction 15-90min under simulated solar irradiation, the place to dye, rhodamine B is completed
Reason.
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| CN107684926A (en) * | 2017-10-31 | 2018-02-13 | 滨州学院 | Handle photochemical catalyst of dyestuff and preparation method thereof in high-salt wastewater |
| CN108339561A (en) * | 2018-02-05 | 2018-07-31 | 燕山大学 | A kind of the graphite phase carbon nitride photochemical catalyst and preparation method of basic bismuth carbonate modification |
| CN108704662A (en) * | 2018-06-22 | 2018-10-26 | 南京白云环境科技集团股份有限公司 | A kind of metalloporphyrin/graphite phase carbon nitride composite photo-catalyst |
| CN109261193A (en) * | 2018-11-09 | 2019-01-25 | 辽宁大学 | Ultrasound-solvent structure Bi2O2CO3/g-C3N4The method and its application of flower-shaped composite photo-catalyst |
| CN111054413A (en) * | 2020-03-05 | 2020-04-24 | 南京师范大学 | Ternary composite multi-effect photocatalyst and preparation method thereof |
| CN112121866A (en) * | 2020-10-09 | 2020-12-25 | 广州大学 | Photocatalyst and preparation method thereof |
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2017
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| Title |
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| QIZHAO WANG,ET.AL.: "Synthesis and characterization of novel PPy/Bi2O2CO3 composite with improved photocatalytic activity for degradation of Rhodamine-B", 《JOURNAL OF ALLOYS AND COMPOUNDS》 * |
| WEI ZHAO,ET.AL.: "Novel Bi2O2CO3/polypyrrole/g-C3N4 nanocomposites with efficient photocatalytic and nonlinear optical properties", 《RSC ADVANCES》 * |
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| CN107684926A (en) * | 2017-10-31 | 2018-02-13 | 滨州学院 | Handle photochemical catalyst of dyestuff and preparation method thereof in high-salt wastewater |
| CN107684926B (en) * | 2017-10-31 | 2020-04-07 | 滨州学院 | Photocatalyst for treating dye in high-salinity wastewater and preparation method thereof |
| CN108339561A (en) * | 2018-02-05 | 2018-07-31 | 燕山大学 | A kind of the graphite phase carbon nitride photochemical catalyst and preparation method of basic bismuth carbonate modification |
| CN108704662A (en) * | 2018-06-22 | 2018-10-26 | 南京白云环境科技集团股份有限公司 | A kind of metalloporphyrin/graphite phase carbon nitride composite photo-catalyst |
| CN109261193A (en) * | 2018-11-09 | 2019-01-25 | 辽宁大学 | Ultrasound-solvent structure Bi2O2CO3/g-C3N4The method and its application of flower-shaped composite photo-catalyst |
| CN109261193B (en) * | 2018-11-09 | 2021-07-20 | 辽宁大学 | Ultrasonic-solvothermal method for synthesizing Bi2O2CO3/g-C3N4Method for preparing flower-shaped composite photocatalyst and application thereof |
| CN111054413A (en) * | 2020-03-05 | 2020-04-24 | 南京师范大学 | Ternary composite multi-effect photocatalyst and preparation method thereof |
| CN111054413B (en) * | 2020-03-05 | 2022-08-26 | 南京师范大学 | Ternary composite multi-effect photocatalyst and preparation method thereof |
| CN112121866A (en) * | 2020-10-09 | 2020-12-25 | 广州大学 | Photocatalyst and preparation method thereof |
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