CN103878000B - A kind of BiOX photocatalyst and preparation method thereof - Google Patents
A kind of BiOX photocatalyst and preparation method thereof Download PDFInfo
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- CN103878000B CN103878000B CN201410106814.3A CN201410106814A CN103878000B CN 103878000 B CN103878000 B CN 103878000B CN 201410106814 A CN201410106814 A CN 201410106814A CN 103878000 B CN103878000 B CN 103878000B
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Abstract
A kind of BiOX photocatalyst take sodium bismuthate as bismuth source, and sodium halide or potassium bromate or cetyl trimethyl ammonium halide or halo cetyl pyridinium or tetrabutyl ammonium halide are halogen source.Halogen source is placed in deionized water, under ultrasound condition, stirs 20min make it dissolve, then sodium bismuthate is added in halogen source, regulate pH; The reactor that this mixed liquor is placed in is reacted, is labeled as respectively by bromine source difference: sodium halide (BiOBr
naBr), potassium bromate (BiOBr
kBrO3), cetyl trimethyl ammonium halide (BiOBr
cTAB), halo cetyl pyridinium (BiOBr
cPB), tetrabutyl ammonium halide (BiOBr
tBB).Described BiOX is applied to visible light photoactivated or rhodamine B degradation (RhB), salicylic acid (SA).All have good stability and visible light catalysis activity, manufacturing process is simple simultaneously, cost is lower.
Description
Technical field
The present invention relates to a kind of visible light-responded photochemical catalyst BiOX and preparation method thereof, and be applied to toxic organic pollutant in degraded environment.
Background technology
Photocatalysis oxidation technique is a kind of new chemical oxidation treatment method, successfully can solve other advanced oxidization methods to remove toxic organics in water body and bring the defect of secondary pollution, have that process operation is simple, easy to operate simultaneously, catalyst low price, remove the advantages such as most organic matter using sunshine as light source.Since the element very important for photocatalysis oxidation technique one is photochemical catalyst, the photochemical catalyst of most study is titanium dioxide, but because its energy gap is comparatively large, visible ray utilization rate is low, photo-generate electron-hole limits it to shortcomings such as recombination rate are high and further applies.Bismuth series photocatalyst has good catalytic performance, particularly in visible-range, has obvious absorption, and this is their outstanding features and advantage.Bismuth series photocatalyst except common oxide, the combined oxidation beyond the region of objective existence that formed with other metals, can also with other nonmetal formation composite oxides, the BiOX such as formed with halogen (BiOX, X=F, Cl, Br, I).
BiOX is a kind of novel semi-conducting material, there is unique electronic structure, good optical property and catalytic performance, can well responding to visible light, thus there is very high catalytic activity, and strengthen gradually along with the increase photocatalytic activity of halogen atom ordinal number, therefore BiOX becomes a new direction of photochemical catalyst research.
There are reports in the application of such photochemical catalyst in degraded water pollutant, this type of document has " harm material journal ", 2009, " taking CTAB as template and bromine source Preparative TLC shape BiOBr photochemical catalyst " (WenzhongWang.PreparationofBiOBrlamellarstructurewithhigh photocatalyticactivitybyCTABasBrsourceandtemplate.Journa lofHazardousMaterials), " catalysis communication " that 167:803 – 809 delivers, 2010, deliver on 11 (5): 460-464 " with by NaBiO
3for BiOX photochemical catalyst and catalytic activity research thereof are prepared in bismuth source " (ChangX.BiOX (X=Cl, Br, I) photocatalystspreparedusingNaBiO
3astheBisource:Characterizationandcatalyticperformance.Ca talysisCommunications), " Solid-state Chemistry ", 2013, " the synthesis of BiOBr that 199:224 – 229 delivers, characterize and photocatalytic activity " (CaimeiFan.Synthesis, characterization, andphotocatalyticpropertiesofBiOBrcatalyst.JournalofSoli dStateChemistry), " materials chemistry ", 2012, 22, 22840 " one-step synthesis oxygen enrichment bismuth oxybromide and structured light catalytic activity characteristic thereof " (JunminNan.Oxygen-richbismuthoxyhalides:generalizedone-po tsynthesis delivered, bandstructuresandvisible-lightphotocatalyticproperties.J ournalofMaterialsChemistry) although the BiOX that these preparation methods obtain has certain photocatalytic activity, but ubiquity use organic compound and is brought secondary pollution or the inefficient problem of visible light photocatalysis.
Summary of the invention
The object of the invention is to overcome the shortcoming in the past preparing BiOX photocatalyst, provide a kind of and adopt sodium bismuthate to be bismuth source, adopt inorganic and organic halogen source to prepare BiOX photocatalyst.
The present invention realizes above-mentioned purpose like this:
A kind of BiOX photocatalyst, with sodium bismuthate (NaBiO
3) be bismuth source, sodium halide (NaX) or potassium bromate (KBrO
3) or cetyl trimethyl ammonium halide (CTAB) or halo cetyl pyridinium (CPB) or tetrabutyl ammonium halide (TBB) prepare the nanoscale BiOX catalyst of high-crystallinity for corresponding halogen source.
The preparation method of BiOX photocatalyst: the deionized water sodium halide of 1mmol or (potassium bromate, cetyl trimethyl ammonium halide, halo cetyl pyridinium, tetrabutyl ammonium halide) being placed in 70mL, constantly stirs 20min and makes it dissolve in ultrasonic procedure; Separately 1mmol sodium bismuthate is added in above-mentioned solution, regulate pH=1; Mixed liquor is placed in the reactor of 100ml, 160-200 DEG C of heating 6-24h.And be labeled as respectively by bromine source difference: sodium halide (BiOBr
naBr), potassium bromate (BiOBr
kBrO3), cetyl trimethyl ammonium halide (BiOBr
cTAB), halo cetyl pyridinium (BiOBr
cPB), tetrabutyl ammonium halide (BiOBr
tBB).
The BiOX that employing said method prepares is for visible light photoactivated rhodamine B degradation (RhB).Concrete response parameter is as follows: RhB initial concentration is 1.37 × 10
-5mol/L; Catalyst amount is 0.5g/L; PH=7; Reaction temperature is room temperature; Light source is visible ray (λ>=420nm, Eav=25000Lux); Reaction time is 90min.The detection method of RhB residual concentration is: 2mL is in 5mL centrifuge tube for the interval sampling of certain reaction time, the centrifugal 5min of 8000r/min, use ultraviolet-uisible spectrophotometer in standing wave length be 554nm(λ=554nm) measure absorbance A.Utilize the absorbance A under the certain reaction time of interval
twith reaction initial absorbance A
0ratio (A
t/ A
0) map with time t, obtain degradation kinetics curve.
The BiOX that employing said method prepares is for visible light photoactivated degraded salicylic acid (SA).Concrete response parameter is as follows: SA initial concentration is 2 × 10
-4mol/L; Catalyst amount is 0.67g/L; Reaction temperature is room temperature; Light source is visible ray (λ>=420nm, Eav=25000Lux).The concentration of SA is detected with high performance liquid chromatography.Utilize the integral area S under the certain reaction time of interval
twith reaction initial absorbance S
0ratio (S
t/ S
0) map with time t, obtain degradation kinetics curve.
The photochemical catalyst adopting the method to prepare all effectively by excited by visible light, can have good stability and visible light catalysis activity, and manufacturing process is simple simultaneously, cost is lower.The BiOX photocatalyst pattern prepared evenly, in lamelliform, and have good visible light activity.Inorganic matter sodium bromide is adopted to be that the bismuth oxybromide (BiOBr) that bromine source is synthesized is better than the photocatalytic activity adopting other bromine sources to synthesize under equal conditions, the bismoclite (BiOCl) prepared under visible light can well sensitization degradation of dye rhodamine B, has investigated by degraded RhB and SA the photocatalytic activity preparing gained bismuth oxyiodide (BiOI).Find through repeatedly repeating preparation experiment (n >=5), adopt this preparation method repeatability and stability fine.
Accompanying drawing explanation
Fig. 1 is the x-ray diffraction pattern (XRD) of the BiOX (Cl, Br, I) that different halogen source prepares.Standard card contrasts, and finds that the standard card that gained bismuth oxybromide is prepared corresponding in the different bromine source of employing five kinds is respectively: BiOBr
naBr(JCPDS:73-2061), BiOBr
kBrO3(JCPDS:85-0862), BiOBr
cTAB(JCPDS:78-0348), BiOBr
cPB(JCPDS:78-0348), BiOBr
tBB(JCPDS:85-0862).The equal peak shape of catalyst is sharp-pointed, and show that catalyst purity is high, degree of crystallinity is high.Sodium chloride is adopted to prepare the corresponding standard card JCPDS:80-0485 of gained BiOCl.KI is adopted to prepare the corresponding standard card JCPDS:73-2062 of gained BiOI.
Fig. 2 is the kinetic curve of bismuth oxybromide rhodamine B degradation (RhB) and salicylic acid (SA) under visible light conditions.
Fig. 3 is the sensitization degradation kinetics curve of bismoclite to rhodamine B (RhB).
Fig. 4 is the kinetic curve of bismuth oxyiodide rhodamine B degradation (RhB) and salicylic acid (SA) under visible light conditions.
Detailed description of the invention
embodiment 1
The sodium bromide getting 0.001mol is dissolved in the deionized water of 70mL, and adds the sodium bismuthate of 0.001mol.Adjust pH=1.16.Be placed in the polytetrafluoroethylene (PTFE) reactor of 100mL, 180 DEG C of reaction 24h, after question response is complete, precipitate suction filtration by gained, carry out alcohol wash and washing respectively, dry 4h for 60 DEG C.
embodiment 2:
The Cetyl bromo-pyridine getting 0.001mol is dissolved in the deionized water of 70mL, and adds the sodium bismuthate of 0.001mol.Adjust pH=1.06.Be placed in the polytetrafluoroethylene (PTFE) reactor of 100mL, 180 DEG C of reaction 12h, after question response is complete, precipitate suction filtration by gained, carry out alcohol wash and washing respectively, dry 4h for 60 DEG C.
embodiment 3:
The softex kw getting 0.001mol is dissolved in the deionized water of 70mL, ultrasonicly makes it dissolve, and adds the sodium bismuthate of 0.001mol.Adjust pH=1.26.Be placed in the polytetrafluoroethylene (PTFE) reactor of 100mL, 160 DEG C of reaction 12h, after question response is complete, precipitate suction filtration by gained, carry out alcohol wash and washing respectively, dry 4h for 60 DEG C.
embodiment 4:
The TBAB getting 0.001mol is dissolved in the deionized water of 70mL, ultrasonicly makes it dissolve, and adds the sodium bismuthate of 0.001mol.Adjust pH=1.32.Be placed in the polytetrafluoroethylene (PTFE) reactor of 100mL, 200 DEG C of reaction 12h, after question response is complete, precipitate suction filtration by gained, carry out alcohol wash and washing respectively, dry 4h for 60 DEG C.
embodiment 5:
The potassium bromate getting 0.001mol is dissolved in the deionized water of 70mL, ultrasonicly makes it dissolve, and adds the sodium bismuthate of 0.001mol.Adjust pH=1.24.Be placed in the polytetrafluoroethylene (PTFE) reactor of 100mL, 180 DEG C of reaction 24h, after question response is complete, precipitate suction filtration by gained, carry out alcohol wash and washing respectively, dry 4h for 60 DEG C.
As shown in Figure 2, BiOBr
naBr, BiOBr
kBrO3, BiOBr
cTAB, BiOBr
cPB, BiOBr
tBBin the dark reaction of 3h, BiOBr is respectively to RhB adsorption rate
naBr(27.36%), BiOBr
kBO(8.15%) BiOBr
cTAB(15.81%), BiOBr
cPB(15.81%), BiOBr
tBB(19.62%).The speed constant of five kinds of catalyst degradations is respectively: BiOBr
naBr(0.1539min
-1), BiOBr
kBO(0.0240min
-1), BiOBr
cTAB(0.0338min
-1), BiOBr
cPB(0.0687min
-1), BiOBr
tBB(0.1161min
-1).The degrading activity order of five kinds of bismuth oxybromide catalyst to SA is respectively: BiOBr
naBr>BiOBr
tBB>BiOBr
cPB>BiOBr
cTAB>BiOBr
kBrO3consistent with the rule of degraded RhB.
embodiment 6:
The sodium chloride getting 0.001mol is dissolved in the deionized water of 70mL, and adds the sodium bismuthate of 0.001mol.Adjust pH=1.20.Be placed in the polytetrafluoroethylene (PTFE) reactor of 100mL, 180 DEG C of reaction 24h, after question response is complete, precipitate suction filtration by gained, carry out alcohol wash and washing respectively, dry 4h for 60 DEG C.
As shown in Figure 3, bismoclite reaction 2hBiOCl adsorbs RhB16.9%; The photodissociation of RhB is 8.81%; The degradation rate constant of RhB is 0.0351min
-1.
embodiment 7:
The sodium iodide getting 0.001mol is dissolved in the deionized water of 70mL, and adds the sodium bismuthate of 0.001mol.Adjust pH=1.24.Be placed in the polytetrafluoroethylene (PTFE) reactor of 100mL, 180 DEG C of reaction 24h, after question response is complete, precipitate suction filtration by gained, carry out alcohol wash and washing respectively, dry 4h for 60 DEG C.
As shown in Figure 4, bismuth oxyiodide reaction 2hBiOCl adsorbs RhB25.67%; The photodissociation of RhB is 8.81%; The degradation rate constant of RhB is 0.0386min
-1.Reaction 14hBiOI can effectively degrade 25.30% SA.
Claims (7)
1. a preparation method for BiOX photocatalyst, is characterized in that, the sodium bromide comprising the steps: to get 0.001mol is dissolved in the deionized water of 70mL, and add the sodium bismuthate of 0.001mol, adjust pH=1.16, be placed in the polytetrafluoroethylene (PTFE) reactor of 100mL, 180 DEG C of reaction 24h, after question response is complete, gained is precipitated suction filtration, carries out alcohol wash and washing respectively, dry 4h for 60 DEG C, obtained bismuth oxybromide, the XRD standard card that this bismuth oxybromide is corresponding is JCPDS:73-2061.
2. a preparation method for BiOX photocatalyst, is characterized in that, the Cetyl bromo-pyridine comprising the steps: to get 0.001mol is dissolved in the deionized water of 70mL, and add the sodium bismuthate of 0.001mol, adjust pH=1.06, be placed in the polytetrafluoroethylene (PTFE) reactor of 100mL, 180 DEG C of reaction 12h, after question response is complete, gained is precipitated suction filtration, carries out alcohol wash and washing respectively, dry 4h for 60 DEG C, obtained bismuth oxybromide, the XRD standard card that this bismuth oxybromide is corresponding is JCPDS:78-0348.
3. the preparation method of a BiOX photocatalyst, it is characterized in that, the softex kw comprising the steps: to get 0.001mol is dissolved in the deionized water of 70mL, ultrasonicly it is made to dissolve, and add the sodium bismuthate of 0.001mol, adjust pH=1.26, be placed in the polytetrafluoroethylene (PTFE) reactor of 100mL, 160 DEG C of reaction 12h, after question response is complete, precipitate suction filtration by gained, carry out alcohol wash and washing respectively, dry 4h for 60 DEG C, obtained bismuth oxybromide, the XRD standard card that this bismuth oxybromide is corresponding is JCPDS:78-0348.
4. the preparation method of a BiOX photocatalyst, it is characterized in that, the TBAB comprising the steps: to get 0.001mol is dissolved in the deionized water of 70mL, ultrasonicly it is made to dissolve, and add the sodium bismuthate of 0.001mol, adjust pH=1.32, be placed in the polytetrafluoroethylene (PTFE) reactor of 100mL, 200 DEG C of reaction 12h, after question response is complete, precipitate suction filtration by gained, carry out alcohol wash and washing respectively, dry 4h for 60 DEG C, obtained bismuth oxybromide, the XRD standard card that this bismuth oxybromide is corresponding is JCPDS:85-0862.
5. the preparation method of a BiOX photocatalyst, it is characterized in that, the potassium bromate comprising the steps: to get 0.001mol is dissolved in the deionized water of 70mL, ultrasonicly it is made to dissolve, and add the sodium bismuthate of 0.001mol, adjust pH=1.24, be placed in the polytetrafluoroethylene (PTFE) reactor of 100mL, 180 DEG C of reaction 24h, after question response is complete, precipitate suction filtration by gained, carry out alcohol wash and washing respectively, dry 4h for 60 DEG C, obtained bismuth oxybromide, the XRD standard card that this bismuth oxybromide is corresponding is JCPDS:85-0862.
6. a preparation method for BiOX photocatalyst, is characterized in that, the sodium chloride comprising the steps: to get 0.001mol is dissolved in the deionized water of 70mL, and add the sodium bismuthate of 0.001mol, adjust pH=1.20, be placed in the polytetrafluoroethylene (PTFE) reactor of 100mL, 180 DEG C of reaction 24h, after question response is complete, gained is precipitated suction filtration, carries out alcohol wash and washing respectively, dry 4h for 60 DEG C, obtained bismoclite, the XRD standard card that this bismoclite is corresponding is JCPDS:80-0485.
7. a preparation method for BiOX photocatalyst, is characterized in that, the sodium iodide comprising the steps: to get 0.001mol is dissolved in the deionized water of 70mL, and add the sodium bismuthate of 0.001mol, adjust pH=1.24, be placed in the polytetrafluoroethylene (PTFE) reactor of 100mL, 180 DEG C of reaction 24h, after question response is complete, gained is precipitated suction filtration, carries out alcohol wash and washing respectively, dry 4h for 60 DEG C, obtained bismuth oxyiodide, the XRD standard card that this bismuth oxyiodide is corresponding is JCPDS:73-2062.
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| CN105289680A (en) * | 2015-11-26 | 2016-02-03 | 常州大学 | Preparation method for visible-light-driven photocatalyst compositing bismuth oxychloride/silver carbonate |
| CN108855011B (en) * | 2016-07-08 | 2020-12-04 | 苏州大学 | Composite material with adsorption-visible light catalytic degradation synergistic effect and application thereof |
| CN106732680A (en) * | 2016-11-29 | 2017-05-31 | 重庆大学 | The method that mixing bromine source prepares microspheroidal BiOBr |
| CN106984338B (en) * | 2017-04-19 | 2019-05-10 | 三峡大学 | It is a kind of to prepare semiconductor BiO using industrial wastewaterxClyThe method of type photochemical catalyst |
| CN107519903B (en) * | 2017-09-09 | 2020-03-31 | 合肥学院 | Bismuth oxybromide-cadmium sulfide nano composite photocatalyst and preparation method thereof |
| CN108355685A (en) * | 2018-03-13 | 2018-08-03 | 江苏建筑职业技术学院 | A kind of preparation method of composite photo-catalyst |
| CN108408773B (en) * | 2018-04-04 | 2020-04-07 | 湘潭大学 | Preparation method and application of BiOCl material |
| CN108483495B (en) * | 2018-04-11 | 2020-04-07 | 湘潭大学 | Preparation method and application of BiOF material |
| CN113926471A (en) * | 2021-10-28 | 2022-01-14 | 盐城工学院 | Preparation method of BiOCl photocatalyst and method for finishing polyester fabric by using BiOCl photocatalyst |
| CN114870873A (en) * | 2022-04-20 | 2022-08-09 | 南昌航空大学 | Method for constructing surface defect photocatalytic material by ion exchange |
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| CN103252244A (en) * | 2013-04-17 | 2013-08-21 | 太原理工大学 | Preparation method and application method of visible-light response type bismuth oxychloride photocatalyst |
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| CN103252244A (en) * | 2013-04-17 | 2013-08-21 | 太原理工大学 | Preparation method and application method of visible-light response type bismuth oxychloride photocatalyst |
Non-Patent Citations (3)
| Title |
|---|
| BiOX (X=Cl, Br, I) photocatalysts prepared using NaBiO3 as the Bi source: Characterization and catalytic performance;Xiaofeng Chang, et al.;《Catalysis Communications》;20091203;第11卷;第460-464页 * |
| Ligand-free one-step synthesis of {001} faceted semiconducting BiOCl single crystals and their photocatalytic activity;Anupam Biswas, et al.;《Crystal Growth and Design》;20131210;第14卷;第236-239页 * |
| Preparation of BiOBr lamellar structure with high photocatalytic activity by CTAB as Br source and template;Meng Shang, et al.;《Journal of Hazardous Materials》;20090123;第167卷;第803-809页 * |
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