CN108620096A - A kind of visible light-responded Ag/Bi3O4Cl composite materials and preparation method and purposes - Google Patents
A kind of visible light-responded Ag/Bi3O4Cl composite materials and preparation method and purposes Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title abstract description 18
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(I) nitrate Inorganic materials [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 40
- 229910052724 xenon Inorganic materials 0.000 claims abstract description 7
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 238000006731 degradation reaction Methods 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 11
- 230000015556 catabolic process Effects 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- YCIHPQHVWDULOY-FMZCEJRJSA-N (4s,4as,5as,6s,12ar)-4-(dimethylamino)-1,6,10,11,12a-pentahydroxy-6-methyl-3,12-dioxo-4,4a,5,5a-tetrahydrotetracene-2-carboxamide;hydrochloride Chemical compound Cl.C1=CC=C2[C@](O)(C)[C@H]3C[C@H]4[C@H](N(C)C)C(=O)C(C(N)=O)=C(O)[C@@]4(O)C(=O)C3=C(O)C2=C1O YCIHPQHVWDULOY-FMZCEJRJSA-N 0.000 claims description 5
- 238000000151 deposition Methods 0.000 claims description 3
- 230000008021 deposition Effects 0.000 claims description 3
- 239000002105 nanoparticle Substances 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 13
- 239000000463 material Substances 0.000 abstract description 6
- 239000004065 semiconductor Substances 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 4
- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract description 4
- 238000010923 batch production Methods 0.000 abstract description 2
- 239000010970 precious metal Substances 0.000 abstract description 2
- 239000000460 chlorine Substances 0.000 description 71
- 229910052709 silver Inorganic materials 0.000 description 17
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 15
- 230000001699 photocatalysis Effects 0.000 description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 10
- 239000000843 powder Substances 0.000 description 10
- 239000007787 solid Substances 0.000 description 10
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 7
- 238000007146 photocatalysis Methods 0.000 description 7
- 239000007788 liquid Substances 0.000 description 6
- 229910002651 NO3 Inorganic materials 0.000 description 5
- 235000019441 ethanol Nutrition 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 238000002604 ultrasonography Methods 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- 239000003643 water by type Substances 0.000 description 5
- AHUBLGVDRKDHAT-UHFFFAOYSA-N [Bi]=O.[Cl] Chemical compound [Bi]=O.[Cl] AHUBLGVDRKDHAT-UHFFFAOYSA-N 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 4
- 229910052801 chlorine Inorganic materials 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 3
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 239000004332 silver Substances 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000003115 biocidal effect Effects 0.000 description 2
- 229910052797 bismuth Inorganic materials 0.000 description 2
- 239000000356 contaminant Substances 0.000 description 2
- 230000000593 degrading effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000011941 photocatalyst Substances 0.000 description 2
- 238000002256 photodeposition Methods 0.000 description 2
- 238000010189 synthetic method Methods 0.000 description 2
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 1
- 229910021607 Silver chloride Inorganic materials 0.000 description 1
- 239000004098 Tetracycline Substances 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- CJJMLLCUQDSZIZ-UHFFFAOYSA-N oxobismuth Chemical compound [Bi]=O CJJMLLCUQDSZIZ-UHFFFAOYSA-N 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- 229910021649 silver-doped titanium dioxide Inorganic materials 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229960002180 tetracycline Drugs 0.000 description 1
- 229930101283 tetracycline Natural products 0.000 description 1
- 235000019364 tetracycline Nutrition 0.000 description 1
- 150000003522 tetracyclines Chemical class 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/06—Halogens; Compounds thereof
-
- 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
- B01J35/20—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state
- B01J35/23—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state in a colloidal state
-
- 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
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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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/344—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electromagnetic wave energy
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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2101/38—Organic compounds containing nitrogen
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract
The invention belongs to technical field of semiconductor material preparation, refer in particular to a kind of visible light-responded Ag/Bi3O4Cl composite materials and preparation method and purposes.By Bi3O4Cl is dissolved in AgNO3After being stirred evenly in solution, 60min is irradiated with 250W xenon lamps, washes, dry to obtain Ag/Bi3O4Cl composite materials.Due to the surface plasma resonance effect (SPR) of precious metals ag, the separative efficiency in light induced electron and hole is effectively raised, photocatalytic degradation capability is further increased, simple for process, reaction cost is low, convenient for batch production, meets environmental-friendly requirement.
Description
Technical field
The invention belongs to technical field of semiconductor material preparation, and Ag/ is synthesized using light deposition synthetic method and two step of hydro-thermal method
Bi3O4Cl photochemical catalysts, for quadracycline performance study of degrading under visible light.
Background technology
In recent years, with economic continuous development, the energy, environmental problem in global range are also increasingly severe.Especially
Large-scale application of the antibiotic in terms of medical personal care articles and animal husbandry, makes the pollution of antibiotic in water body environment have become
The hot issue of current research.The current solar energy that develops and utilizes is one of the significant challenge for solving current environmental crisis, in recent years
Come, photocatalysis degradation organic contaminant has been generally considered solution because having many advantages, such as that energy saving, efficient, contaminant degradation is thorough
The important channel of certainly current water body orgnic compound pollution problem, photocatalysis technology can utilize green and free of contamination sunlight
The degradation of organic pollutants in water body can be realized, to achieve the purpose that improve environment and utilize solar energy, it is known that too
In solar spectrum, ultraviolet light only accounts for 5%, and the ratio of visible light is up to 43%, therefore, develop can practical application visible light
The semiconductor light-catalyst of response is the hot issue of current photocatalysis research field.
Recently, a kind of environmentally protective semiconductor chlorine oxygen bismuth (Bi3O4Cl), due to its good chemistry and thermal stability, low
Honest and clean cost, it is safe and non-toxic the features such as the concern of researchers is gradually caused in photocatalysis field；Chlorine oxygen bismuth (Bi3O4Cl) it is
A kind of important metal oxide, band gap width are 2.7eV or so, are a kind of good visible light-responded materials, currently, chlorine oxygen
Bismuth (Bi3O4Cl) research in terms of photocatalytic pollutant degradation has been reported；But single chlorine oxygen bismuth (Bi3O4Cl) material
Material is since the shortcomings of its poor degradation property and its poor photo-generate electron-hole separative efficiency leads to its photocatalytic activity and can
Light-exposed utilization ratio is unsatisfactory, in recent years, structure chlorine oxygen bismuth (Bi3O4Cl) composite system is a kind of effective strategy
It goes to improve its photocatalysis performance, that is because it can effectively improve the separation of photo-generate electron-hole pair.On the other hand, silver-colored
(Ag), as a kind of important noble metal, now research finds that a small amount of Ag and semiconductors coupling can significantly enhance photocatalysis
Performance, such as：Ag/AgCl, Ag/Bi2WO6, Ag/TiO2And Ag/Bi3TaO7Deng, however, up to the present there are no Ag with
Bi3O4Cl is compounded to form the preparation of hetero-junctions and the report of photocatalytic applications.
Invention content
The purpose of the present invention is to provide a kind of simple and quick Ag/Bi3O4The synthetic method of Cl composite materials, this method
Using five nitric hydrate bismuths, ammonium chloride and silver nitrate as raw material, the Ag/ of hydration method and the response of Photodeposition synthesizing visible light is utilized
Bi3O4Cl composite photocatalyst materials.
A kind of visible light-responded Ag/Bi provided by the invention3O4The preparation method of Cl composite materials, it is characterised in that packet
Include following steps：
Step 1：Bi3O4The preparation of Cl nanometer sheets
First by 0.485g Bi (NO3)3·5H2O ultrasonic disperses stir ultrasound 10min in 10mL ethylene glycol, obtain molten
Liquid A.Secondly by 0.018g NH4Cl, which is dissolved in 25mL deionized waters, obtains solution B, and solution B is slowly added in above-mentioned solution A,
It generates white turbid to be transferred in 50mL reaction kettles, 160 DEG C of hydro-thermal 12h.It waits for that reaction kettle is cooled to room temperature, sample is washed with water and ethyl alcohol,
60 DEG C of drying obtain solid powder C.Finally, solid powder C is roasted into 5h under 500 DEG C of Muffle furnaces, 5 DEG C/min of heating rate.
Finally obtain Bi3O4Cl nanometer sheets.
Step 2：Ag/Bi3O4The preparation of Cl composite materials
By Bi3O4Cl is dissolved in AgNO3After being stirred evenly in solution, 60min is irradiated with 250W xenon lamps, washes, dry
Ag/Bi3O4Cl composite materials.
Further, Bi3O4Cl and AgNO3The mass volume ratio of solution is 0.5g：5ml, AgNO3Solution it is a concentration of
1mg/ml。
Further, mixing time 30min.
Further, washing, which refers to, is washed with deionized water 3 times, and drying temperature is 60 DEG C.
Further, in composite material, Ag and Bi3O4The mass ratio of Cl is 0.01:1.
Advantageous effect
Ag/Bi is synthesized using hydro-thermal method and Photodeposition3O4Cl composite photo-catalysts, hydrochloric acid Fourth Ring of degrading under visible light
Element shows excellent photocatalytic activity；The difficult point of the present invention is silver nano-grain being deposited on Bi3O4In Cl nanometer sheets, this
Invention captures this difficult point by the method for light deposition, due to the surface plasma resonance effect (SPR) of precious metals ag, effectively
The separative efficiency for improving light induced electron and hole further increases photocatalytic degradation capability, and simple for process, reaction cost is low,
Convenient for batch production, meet environmental-friendly requirement.
Description of the drawings
Fig. 1 (a) is the x-ray diffraction pattern (XRD) of sample prepared by the present invention；Fig. 1 (b) is sample prepared by the present invention
Energy spectrum analysis figure (EDX)；It can be seen that pure Bi from the test result of XRD3O4The diffraction maximum of Cl and standard diagram (JCPDS,
No.36-0760) corresponding, since the content of silver is smaller, so not finding the diffraction maximum of silver.It can from the test result of EDX
To detect Bi, O, Cl, Ag element, illustrate that Ag nano particles are successfully deposited on Bi3O4On the surface of Cl.
Fig. 2 is the x-ray photoelectron spectroscopy figure (XPS) of sample prepared by the present invention, and test result shows prepared sample
Including element Bi, O, Cl, Ag, illustrate that XPS collection of illustrative plates shows that it has all elements of synthesized sample, this result is demonstrate,proved indirectly
Bright Ag nano particles are successfully deposited on Bi3O4On the surface of Cl.
Fig. 3 shows Bi3O4Cl, 0.5wt%Ag/Bi3O4Cl, 1wt%Ag/Bi3O4Cl, 3wt%Ag/Bi3O4Cl and 5wt%
Ag/Bi3O4Degradation time-degradation rate relational graph of Cl photochemical catalysts photocatalytic degradation quadracycline solution under visible light.From
It can be seen from the figure that, quadracycline itself can be stabilized under visible light illumination, pure Bi3O4Cl under visible light 120
Degradation rate only has 61% under minute, however compared to pure Bi3O4Cl, Ag/Bi3O4Cl composite materials are degraded salt under visible light
The photocatalytic activity of sour tetracycline significantly improves.As load 1wt%Bi3O4When Cl, photocatalytic degradation quadracycline activity is most
Height, lower degradation rate can reach 94.2% within 120 minutes.
Specific implementation mode
Embodiment 1
Step 1：Bi3O4The preparation of Cl nanometer sheets
First by 0.485g Bi (NO3)3·5H2O ultrasonic disperses stir ultrasound 10min in 10mL ethylene glycol, obtain molten
Liquid A.Secondly by 0.018g NH4Cl, which is dissolved in 25mL deionized waters, obtains solution B, and solution B is slowly added in above-mentioned solution A,
It generates white turbid to be transferred in 50mL reaction kettles, 160 DEG C of hydro-thermal 12h.It waits for that reaction kettle is cooled to room temperature, sample is washed with water and ethyl alcohol,
Drying obtains solid powder C.Finally, solid powder C is roasted into 5h under 500 DEG C of Muffle furnaces, 5 DEG C/min of heating rate.Finally
Obtain Bi3O4Cl nanometer sheets.
Step 2：Ag/Bi3O4The preparation of Cl composite materials
By Bi3O4Cl is dissolved in AgNO3After being stirred evenly in solution, 60min is irradiated with 250W xenon lamps, washes, dry
Ag/Bi3O4Cl composite materials.
Further, Bi3O4Cl and AgNO3The mass volume ratio of solution is 0.5g:2.5ml, AgNO3Solution it is a concentration of
1mg/ml。
Further, mixing time 30min.
Further, washing, which refers to, is washed with deionized water 3 times, and drying temperature is 60 DEG C.
Further, in composite material, Ag and Bi3O4The mass ratio of Cl is 0.005:1, it is calculated as 0.5wt%Ag/
Bi3O4Cl。
Embodiment 2
Step 1：Bi3O4The preparation of Cl nanometer sheets
First by 0.485g Bi (NO3)3·5H2O ultrasonic disperses stir ultrasound 10min in 10mL ethylene glycol, obtain molten
Liquid A.Secondly by 0.018g NH4Cl, which is dissolved in 25mL deionized waters, obtains solution B, and solution B is slowly added in above-mentioned solution A,
It generates white turbid to be transferred in 50mL reaction kettles, 160 DEG C of hydro-thermal 12h.It waits for that reaction kettle is cooled to room temperature, sample is washed with water and ethyl alcohol,
Drying obtains solid powder C.Finally, solid powder C is roasted into 5h under 500 DEG C of Muffle furnaces, 5 DEG C/min of heating rate.Finally
Obtain Bi3O4Cl nanometer sheets.
Step 2：Ag/Bi3O4The preparation of Cl composite materials
By Bi3O4Cl is dissolved in AgNO3After being stirred evenly in solution, 60min is irradiated with 250W xenon lamps, washes, dry
Ag/Bi3O4Cl composite materials.
Further, Bi3O4Cl and AgNO3The mass volume ratio of solution is 0.5g：5ml, AgNO3Solution it is a concentration of
1mg/ml。
Further, mixing time 30min.
Further, washing, which refers to, is washed with deionized water 3 times, and drying temperature is 60 DEG C.
Further, in composite material, Ag and Bi3O4The mass ratio of Cl is 0.01:1, it is calculated as 1wt%Ag/Bi3O4Cl。
Embodiment 3
Step 1：Bi3O4The preparation of Cl nanometer sheets
First by 0.485g Bi (NO3)3·5H2O ultrasonic disperses stir ultrasound 10min in 10mL ethylene glycol, obtain molten
Liquid A.Secondly by 0.018g NH4Cl, which is dissolved in 25mL deionized waters, obtains solution B, and solution B is slowly added in above-mentioned solution A,
It generates white turbid to be transferred in 50mL reaction kettles, 160 DEG C of hydro-thermal 12h.It waits for that reaction kettle is cooled to room temperature, sample is washed with water and ethyl alcohol,
Drying obtains solid powder C.Finally, solid powder C is roasted into 5h under 500 DEG C of Muffle furnaces, 5 DEG C/min of heating rate.Finally
Obtain Bi3O4Cl nanometer sheets.
Step 2：Ag/Bi3O4The preparation of Cl composite materials
By Bi3O4Cl is dissolved in AgNO3After being stirred evenly in solution, 60min is irradiated with 250W xenon lamps, washes, dry
Ag/Bi3O4Cl composite materials.
Further, Bi3O4Cl and AgNO3The mass volume ratio of solution is 0.5g:15ml, AgNO3Solution it is a concentration of
1mg/ml。
Further, mixing time 30min.
Further, washing, which refers to, is washed with deionized water 3 times, and drying temperature is 60 DEG C.
Further, in composite material, Ag and Bi3O4The mass ratio of Cl is 0.03:1, it is calculated as 3wt%Ag/Bi3O4Cl。
Embodiment 4
Step 1：Bi3O4The preparation of Cl nanometer sheets
First by 0.485g Bi (NO3)3·5H2O ultrasonic disperses stir ultrasound 10min in 10mL ethylene glycol, obtain molten
Liquid A.Secondly by 0.018g NH4Cl, which is dissolved in 25mL deionized waters, obtains solution B, and solution B is slowly added in above-mentioned solution A,
It generates white turbid to be transferred in 50mL reaction kettles, 160 DEG C of hydro-thermal 12h.It waits for that reaction kettle is cooled to room temperature, sample is washed with water and ethyl alcohol,
Drying obtains solid powder C.Finally, solid powder C is roasted into 5h under 500 DEG C of Muffle furnaces, 5 DEG C/min of heating rate.Finally
Obtain Bi3O4Cl nanometer sheets.
Step 2：Ag/Bi3O4The preparation of Cl composite materials
By Bi3O4Cl is dissolved in AgNO3After being stirred evenly in solution, 60min is irradiated with 250W xenon lamps, washes, dry
Ag/Bi3O4Cl composite materials.
Further, Bi3O4Cl and AgNO3The mass volume ratio of solution is 0.5g:25ml, AgNO3Solution it is a concentration of
1mg/ml。
Further, mixing time 30min.
Further, washing, which refers to, is washed with deionized water 3 times, and drying temperature is 60 DEG C.
Further, in composite material, Ag and Bi3O4The mass ratio of Cl is 0.05:1, it is calculated as 5wt%Ag/Bi3O4Cl。
Embodiment 5
By the Bi of above-mentioned preparation3O4Cl, 0.5wt%Ag/Bi3O4Cl, 1wt%Ag/Bi3O4Cl, 3wt%Ag/Bi3O4Cl、
5wt%Ag/Bi3O4Cl samples carry out following degradation experiment respectively：
Step 1：The Preparatory work of experiment stage
It weighs 0.05g catalyst respectively to be added in 100ml TC (10mg/L) solution, ultrasonic 5min is to be used.
Step 2：The experimentation stage
Sample in step 1 is put into photocatalysis apparatus, dark reaction 30min, takes first sample, taken later every 20min
One sample, coreaction 120min.
Step 3：The experiment test stage
Gained sample supernatant in step 2 is subjected to the ultraviolet test of liquid, and drafting pattern 3.
Claims (6)
1. a kind of visible light-responded Ag/Bi3O4Cl composite materials, Ag nanoparticle depositions are in Bi3O4On the surface of Cl, feature exists
In preparing with the following method：By Bi3O4Cl is dissolved in AgNO3After being stirred evenly in solution, 60min is irradiated with 250W xenon lamps,
It washes, dry to obtain Ag/Bi3O4Cl composite materials.
2. a kind of visible light-responded Ag/Bi as described in claim 13O4Cl composite materials, which is characterized in that Bi3O4Cl with
AgNO3The mass volume ratio of solution is 0.5g：5ml, AgNO3A concentration of 1mg/ml of solution.
3. a kind of visible light-responded Ag/Bi as described in claim 13O4Cl composite materials, which is characterized in that mixing time is
30min。
4. a kind of visible light-responded Ag/Bi as described in claim 13O4Cl composite materials, which is characterized in that further, water
It washes finger to be washed with deionized water 3 times, drying temperature is 60 DEG C.
5. a kind of visible light-responded Ag/Bi as described in claim 13O4Cl composite materials, which is characterized in that in composite material,
Ag and Bi3O4The mass ratio of Cl is 0.01:1.
6. a kind of visible light-responded Ag/Bi as described in any in claim 1-53O4The purposes of Cl composite materials, in visible light
Lower degradation quadracycline, lower degradation rate reaches 94.2% within 120 minutes.
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