CN109158124A - A kind of carbonitride and BiOX composite photocatalyst material and preparation method thereof - Google Patents
A kind of carbonitride and BiOX composite photocatalyst material and preparation method thereof Download PDFInfo
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- CN109158124A CN109158124A CN201811163903.6A CN201811163903A CN109158124A CN 109158124 A CN109158124 A CN 109158124A CN 201811163903 A CN201811163903 A CN 201811163903A CN 109158124 A CN109158124 A CN 109158124A
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- 239000000463 material Substances 0.000 title claims abstract description 44
- 239000002131 composite material Substances 0.000 title claims abstract description 39
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims abstract description 22
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- IOLCXVTUBQKXJR-UHFFFAOYSA-M potassium bromide Chemical compound [K+].[Br-] IOLCXVTUBQKXJR-UHFFFAOYSA-M 0.000 claims abstract description 10
- 239000004094 surface-active agent Substances 0.000 claims abstract description 10
- 229940106691 bisphenol a Drugs 0.000 claims abstract description 8
- 239000001103 potassium chloride Substances 0.000 claims abstract description 7
- 235000011164 potassium chloride Nutrition 0.000 claims abstract description 7
- 239000011259 mixed solution Substances 0.000 claims abstract description 5
- 229910052794 bromium Inorganic materials 0.000 claims abstract description 4
- 229910052740 iodine Inorganic materials 0.000 claims abstract description 4
- 239000002957 persistent organic pollutant Substances 0.000 claims abstract description 4
- 230000003197 catalytic effect Effects 0.000 claims abstract description 3
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 3
- PPNKDDZCLDMRHS-UHFFFAOYSA-N dinitrooxybismuthanyl nitrate Chemical class [Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PPNKDDZCLDMRHS-UHFFFAOYSA-N 0.000 claims abstract description 3
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 claims abstract description 3
- 150000005846 sugar alcohols Polymers 0.000 claims abstract description 3
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 44
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 claims description 11
- 238000001354 calcination Methods 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 230000015556 catabolic process Effects 0.000 claims description 6
- 238000006731 degradation reaction Methods 0.000 claims description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 5
- 235000019441 ethanol Nutrition 0.000 claims description 5
- 239000001301 oxygen Substances 0.000 claims description 5
- 229910052760 oxygen Inorganic materials 0.000 claims description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- 229910052797 bismuth Inorganic materials 0.000 claims description 4
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 4
- 229910052736 halogen Inorganic materials 0.000 claims description 4
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 4
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 3
- 229920000877 Melamine resin Polymers 0.000 claims description 3
- WOWHHFRSBJGXCM-UHFFFAOYSA-M cetyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCC[N+](C)(C)C WOWHHFRSBJGXCM-UHFFFAOYSA-M 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 150000002367 halogens Chemical class 0.000 claims description 3
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 3
- 229920002401 polyacrylamide Polymers 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 claims description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 2
- TVXBFESIOXBWNM-UHFFFAOYSA-N Xylitol Natural products OCCC(O)C(O)C(O)CCO TVXBFESIOXBWNM-UHFFFAOYSA-N 0.000 claims description 2
- HIVLDXAAFGCOFU-UHFFFAOYSA-N ammonium hydrosulfide Chemical compound [NH4+].[SH-] HIVLDXAAFGCOFU-UHFFFAOYSA-N 0.000 claims description 2
- 239000004202 carbamide Substances 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 238000005119 centrifugation Methods 0.000 claims description 2
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- -1 halogen Bismuth oxide Chemical class 0.000 claims description 2
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims description 2
- HEBKCHPVOIAQTA-UHFFFAOYSA-N meso ribitol Natural products OCC(O)C(O)C(O)CO HEBKCHPVOIAQTA-UHFFFAOYSA-N 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 239000000811 xylitol Substances 0.000 claims description 2
- HEBKCHPVOIAQTA-SCDXWVJYSA-N xylitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)CO HEBKCHPVOIAQTA-SCDXWVJYSA-N 0.000 claims description 2
- 235000010447 xylitol Nutrition 0.000 claims description 2
- 229960002675 xylitol Drugs 0.000 claims description 2
- 229910000416 bismuth oxide Inorganic materials 0.000 claims 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims 1
- 230000003760 hair shine Effects 0.000 abstract description 6
- 238000000034 method Methods 0.000 abstract description 5
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 3
- 230000004298 light response Effects 0.000 abstract description 3
- 238000000227 grinding Methods 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 abstract 1
- 229940073609 bismuth oxychloride Drugs 0.000 description 7
- BWOROQSFKKODDR-UHFFFAOYSA-N oxobismuth;hydrochloride Chemical compound Cl.[Bi]=O BWOROQSFKKODDR-UHFFFAOYSA-N 0.000 description 7
- 230000001699 photocatalysis Effects 0.000 description 7
- 238000006555 catalytic reaction Methods 0.000 description 6
- 238000007146 photocatalysis Methods 0.000 description 6
- 238000005286 illumination Methods 0.000 description 5
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 229910002651 NO3 Inorganic materials 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 235000011187 glycerol Nutrition 0.000 description 2
- 125000005843 halogen group Chemical group 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(III) oxide Inorganic materials O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000013507 mapping Methods 0.000 description 1
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 1
- 229940012189 methyl orange Drugs 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000006213 oxygenation reaction Methods 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
Classifications
-
- 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- B01J35/39—
-
- 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
- C02F2101/34—Organic compounds containing oxygen
- C02F2101/345—Phenols
-
- 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
Abstract
The invention belongs to photocatalyst technology field, specially a kind of carbonitride and BiOX composite photocatalyst material and preparation method thereof.Composite photocatalyst material of the invention has layer structure, wherein carbonitride is denoted as g-C3N4, BiOX is denoted as BiOXaYb, X, Y=Cl, Br or I, and X ≠ Y, a+b=1;The present invention is by g-C3N4Presoma be put in Muffle furnace calcine be made g-C3N4, then mix with five water bismuth nitrates, surfactant and polyalcohol;It is added two kinds in potassium chloride, potassium bromide and liquor kalii iodide;Adjust the pH of mixed solution;Gained sample is filtered or is centrifuged, is washed to neutrality, g-C is made in dry, grinding3N4With BiOXaYbComposite photocatalyst material.The composite material has the characteristics that efficient visible light response, under the conditions of visible light shines, can efficient catalytic degrade in dirty (useless) water using bisphenol-A as the emerging organic pollutant of representative.Preparation method simple process of the present invention, operation are easy, and yield is high, low energy consumption, and preparation condition is mild, environmental-friendly.
Description
Technical field
The invention belongs to photocatalyst technology fields, and in particular to a kind of photochemical catalyst and preparation method thereof, more particularly to
A kind of carbonitride (g-C3N4) and BiOX (BiOXaYb) composite photocatalyst material and preparation method thereof.
Background technique
As the Typical Representative in bismuth oxyhalide, bismuth oxychloride (BiOCl) is due to its stable chemical property, nontoxic
Property, corrosion resistance, outstanding spectrochemical property and have layer structure and be widely used in photocatalysis field.But
BiOCl, only to ultraviolet light response, greatly limits its practical application value due to its wider band gap.And introduce halogen atom
(such as Br, I) can further improve the response to visible light.Meanwhile the non-metal semiconductive carbonitride (g-C of graphite-phase3N4) because
The response to visible light is shown with relatively narrow band gap (about 2.7eV), is also applied due to its presoma cheap and easy to get
It has a extensive future.However, g-C3N4Photo-generate electron-hole itself is easily compound, and photocatalytic activity will receive limitation.Therefore, BiOCl, halogen
Plain atom and g-C3N4Compound efficient response to visible light can be achieved.
Traditional BiOCl preparation method usually requires high temperature and pressure, such as hydro-thermal method, and yield is lower, consumes energy higher.South China
Polytechnics reports through dinectly bruning Bi2O3And C3N4Presoma and obtain a kind of g-C3N4/ bismuth system oxide is compound can
Light-exposed catalyst can remove nearly 70% methyl orange (number of patent application: 201410809217.7) in 300 min;Tianjin science and technology is big
Report using microwave method prepare a kind of high performance BiOCl/BiOBr catalysis material (number of patent application:
201610834479.8);Harbin Institute of Technology reports using surfactant, successfully makes under 160 DEG C of hydrothermal condition
Standby Lacking oxygen high performance out enriches BiOCl-g-C3N4Hetero-junctions, and point out that the addition of surfactant can significantly increase
Oxygenation vacancy (Applied Catalysis B:Environmental, 2018,220,290-302).It can be seen that BiOCl,
Halogen atom, surfactant and g-C3N4The respective party face of visible light is played an important role improving catalysis material.But
Up to the present, high-performance, the g-C with abundant Lacking oxygen are realized using surfactant3N4With BiOXaYbComposite material
Preparation, there has been no relevant document reports.
Summary of the invention
The present invention is intended to provide a kind of simple process, operation be easy, high yield, low energy consumption, preparation condition is mild, environment is friendly
Composite photocatalyst material and preparation method thereof good and with efficient visible light response.
Composite photocatalyst material provided by the invention is a kind of carbonitride (g-C3N4) and BiOX (BiOXaYb) compound
Catalysis material, X, Y=Cl, Br or I, and+b=1 X ≠ Y, a;The composite photocatalyst material has layer structure.
Above-mentioned g-C3N4With BiOXaYbComposite photocatalyst material, wherein bismuth, oxygen, halogen, carbon and nitrogen each element high uniformity divide
Cloth, and material has Lacking oxygen abundant.
G-C provided by the invention3N4With BiOXaYbCompound catalysis material, can be used for photocatalytic degradation municipal sewage,
Emerging organic pollutant in industrial wastewater, polluted river water, is with a wide range of applications.
The present invention also provides above-mentioned g-C3N4With BiOXaYbThe preparation method of compound catalysis material, specific steps are such as
Under:
(1) by quantitative g-C3N4Presoma be put in Muffle furnace, carry out calcination processing again;
It (2) again will be through the g-C of step (1) calcination processing3N4It is dissolved in water, obtains g-C3N4Aqueous solution;Ultrasonic disperse is uniform;
(3) under the conditions of 40 DEG C ~ 100 DEG C of low temperature, by the solution of step (2) and five water bismuth nitrate (Bi (NO3)3·5H2O),
Surfactant and polyalcohol are uniformly mixed;
(4) be added into the solution of step (3) potassium chloride, any two kinds in potassium bromide and liquor kalii iodide it is uniformly mixed molten
Liquid;
(5) pH of step (4) mixed solution is adjusted to 7.5 ~ 11.5, reaction 10min ~ for 24 hours;
(6) the resulting sample of step (5) is filtered or centrifugation, washing to neutrality, drying is ground to get g-C3N4With
BiOClxI1-xComposite photocatalyst material.
In step (1), the g-C3N4Presoma be one of urea, melamine, dicyandiamide and sulphur ammonium etc. or
Several, the quality of the presoma is 0.1g ~ 100g.The temperature of the calcination processing is 350 DEG C ~ 800 DEG C, and calcination time is
0.1h~ 100h;Preferred calcination temperature is 600 DEG C ~ 800 DEG C, and calcination time is 1h ~ 30h.
In step (2), the g-C3N4The concentration of aqueous solution be 0.5g/L ~ 100g/L, ultrasonic time be 10min ~
24h;It is preferred that g-C3N4The concentration of aqueous solution is 5g/L ~ 60g/L, and ultrasonic time is 1h ~ 20h.
In step (3), the quality of the five water bismuth nitrates is 0.1g ~ 100g, and the surfactant is polyethylene
Pyrrolidones (PVP), lauryl sodium sulfate, xylitol, polyacrylamide (PAM), cetyl trimethylammonium bromide
(CTAB) and one or more of hexadecyltrimethylammonium chloride (CTAC) etc., dosage is 0.01g ~ 10g, and described is more
First alcohol is one or more of ethyl alcohol, ethylene glycol, diethylene glycol (DEG), isopropanol and glycerine etc., and dosage is 1mL ~ 200mL.
In step (4), the concentration of the potassium chloride, potassium bromide and potassium iodide is all 0.1g/L ~ 50g/L.
The range of pH described in step (5) is 7.5 ~ 11.5, and the reaction time is 10min ~ for 24 hours.
Carbonitride (g-C prepared by the present invention3N4) and BiOX (BiOXaYb) composite photocatalyst material, it is shone in visible light
Under the conditions of, can efficient catalytic degrade in dirty (useless) water using bisphenol-A as the emerging organic pollutant of representative.
The invention has the benefit that
Preparation method simple process of the present invention, operation are easy, and yield is high, low energy consumption, and preparation condition is mild, environmental-friendly.Preparation
Composite photocatalyst material activity it is higher, have broader practice prospect.
Detailed description of the invention
Fig. 1 is g-C prepared by embodiment 13N4With BiOXaYbThe scanning electron microscope (SEM) of composite photocatalyst material
Structure chart.
Fig. 2 is g-C prepared by embodiment 13N4With BiOXaYbThe transmission electron microscope (TEM) of composite photocatalyst material
Structure chart.
Fig. 3 is g-C prepared by embodiment 13N4With BiOXaYbThe element mapping distribution map of composite photocatalyst material.
Fig. 4 is g-C prepared by embodiment 13N4With BiOXaYbComposite photocatalyst material under visible light illumination drop by photocatalysis
Solve bisphenol-A.
Fig. 5 is g-C prepared by embodiment 23N4With BiOXaYbComposite photocatalyst material under visible light illumination drop by photocatalysis
Solve bisphenol-A.
Fig. 6 is g-C prepared by embodiment 33N4With BiOXaYbComposite photocatalyst material under visible light illumination drop by photocatalysis
Solve bisphenol-A.
Fig. 7 is g-C prepared by embodiment 43N4With BiOXaYbComposite photocatalyst material under visible light illumination drop by photocatalysis
Solve bisphenol-A.
Fig. 8 is g-C prepared by embodiment 53N4With BiOXaYbComposite photocatalyst material under visible light illumination drop by photocatalysis
Solve bisphenol-A.
Specific embodiment
Below in conjunction with specific example, explanation that the present invention is further elaborated, but the present invention be not limited in it is following
Embodiment.
Embodiment 1
G-C of the invention3N4With BiOXaYbThe preparation method of composite photocatalyst material, comprising the following steps:
By 2gg-C3N4Presoma melamine be put in crucible with cover, calcine 2 h under the conditions of 550 DEG C with Muffle furnace.
By 0.3 g g-C3N430 min of ultrasound after being mixed with the deionized water of 25 mL, to g-C under the conditions of 80 DEG C3N4Aqueous solution in
Sequentially add 5.8gBi (NO3)3·5H230min is mixed after O, 0.5g PVP and 25mL glycerine, then 0.67gKCl is added dropwise
With the 100mL mixed solution of the total 12mmol of 0.50g KI(KCl and KI), is adjusted under the conditions of pH is 9.0,80 DEG C and continued instead with ammonium hydroxide
Answer 1h.By sample filtering and washing 3 times after reaction, then dry, grinding is to get g-C3N4With BiOXaYbComposite photocatalyst material
(Fig. 1, Fig. 2 and Fig. 3).
The composite photocatalyst material is used to degrade 10 mg/L bisphenol-A (BPA) solution, when visible light shines 30 min,
The degradation rate of BPA is 97.4 %(Fig. 4).
Embodiment 2
G-C in the present embodiment, in step (2)3N4Quality be 0.2 g, other each steps are same as Example 1.
The composite photocatalyst material is used to degrade 10 mg/LBPA solution, when visible light shines 30 min, the degradation of BPA
Rate is 96.8 %(Fig. 5).
Embodiment 3
G-C in the present embodiment, in step (2)3N4Quality be 0.4 g, other each steps are same as Example 1.
The composite photocatalyst material is used to degrade 10 mg/LBPA solution, when visible light shines 30 min, the degradation of BPA
Rate is 93.6 %(Fig. 6).
Embodiment 4
In the present embodiment, surfactant PVP is not added in step (3), other each steps are same as Example 1.
The composite photocatalyst material is used to degrade 10 mg/LBPA solution, when visible light shines 60 min, the degradation of BPA
Rate is 38.8 %(Fig. 7).
Embodiment 5
In the present embodiment, do not add potassium iodide in step (4), i.e., 0.895g KCl(12 mmoL be only added) 100mL solution,
Other each steps are same as Example 1.
The composite photocatalyst material is used to degrade 10 mg/LBPA solution, when visible light shines 60 min, the degradation of BPA
Rate is only 4.4 %(Fig. 8).
Claims (8)
1. a kind of carbonitride and BiOX composite photocatalyst material have layer structure, wherein carbonitride g-C3N4, halogen
Bismuth oxide is BiOXaYb, X, Y=Cl, Br or I, and+b=1 X ≠ Y, a.
2. carbonitride according to claim 1 and BiOX composite photocatalyst material, which is characterized in that bismuth in material,
Oxygen, halogen, carbon and the distribution of nitrogen each element high uniformity.
3. a kind of preparation method of carbonitride as described in claim 1 and BiOX composite photocatalyst material, feature exist
In, the specific steps are as follows:
(1) by quantitative g-C3N4Presoma is put in Muffle furnace, carries out calcination processing again;
It (2) will be through the g-C of step (1) calcination processing3N4It is dissolved in water, obtains g-C3N4Aqueous solution;Ultrasonic disperse is uniform;
(3) under the conditions of 40 DEG C ~ 100 DEG C of low temperature, by the solution of step (2) and five water bismuth nitrates, surfactant and polynary
Alcohol is uniformly mixed;
(4) potassium chloride is added into the solution of step (3), any two uniformly mixed solution in potassium bromide and liquor kalii iodide;
(5) pH of step (4) mixed solution is adjusted to 7.5 ~ 11.5, reaction 10min ~ for 24 hours;
(6) the resulting sample of step (5) is filtered or centrifugation, washing to neutrality, drying is ground to get g-C3N4With BiOXaYb's
Composite photocatalyst material.
4. the preparation method of carbonitride according to claim 3 and BiOX composite photocatalyst material, feature exist
In, in step (1), the g-C3N4Presoma be one or more of urea, melamine, dicyandiamide and sulphur ammonium, should
The quality of presoma is 0.1g ~ 100g;The calcination processing temperature be 350 DEG C ~ 800 DEG C, calcination time be 0.1h ~
100h。
5. the preparation method of carbonitride according to claim 3 and BiOX composite photocatalyst material, feature exist
In, in step (2), the g-C3N4The concentration of aqueous solution is 0.5g/L ~ 100g/L, and ultrasonic time is 10min ~ for 24 hours.
6. the preparation method of carbonitride according to claim 3 and BiOX composite photocatalyst material, feature exist
In in step (3), the quality of the five water bismuth nitrate is 0.1g ~ 100g;The surfactant be polyvinylpyrrolidone,
In lauryl sodium sulfate, xylitol, polyacrylamide, cetyl trimethylammonium bromide and hexadecyltrimethylammonium chloride
One or more, dosage be 0.01g ~ 10g;The polyalcohol is ethyl alcohol, ethylene glycol, diethylene glycol (DEG), isopropanol and the third three
One or more of alcohol etc., dosage are 1mL ~ 200mL.
7. the preparation method of carbonitride according to claim 3 and BiOX composite photocatalyst material, feature exist
In in step (4), the concentration of the potassium chloride, potassium bromide and potassium iodide is all 0.1g/L ~ 50g/L.
8. carbonitride as described in claim 1 and BiOX composite photocatalyst material, in dirty (useless) water of efficient catalytic degradation
In using bisphenol-A as the application in the emerging organic pollutant of representative.
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CN112023972A (en) * | 2020-09-03 | 2020-12-04 | 上海应用技术大学 | Composite photocatalytic material and preparation method and application thereof |
CN112028038A (en) * | 2020-09-01 | 2020-12-04 | 华东理工大学 | Preparation method and application of alkalized carbon nitride nanotube |
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