CN110270354A - A kind of preparation process of the excellent novel BiOX solid solution of photocatalysis performance - Google Patents
A kind of preparation process of the excellent novel BiOX solid solution of photocatalysis performance Download PDFInfo
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- CN110270354A CN110270354A CN201810216229.7A CN201810216229A CN110270354A CN 110270354 A CN110270354 A CN 110270354A CN 201810216229 A CN201810216229 A CN 201810216229A CN 110270354 A CN110270354 A CN 110270354A
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- 239000006104 solid solution Substances 0.000 title claims abstract description 52
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 238000007146 photocatalysis Methods 0.000 title claims abstract description 11
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 11
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000000243 solution Substances 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000002604 ultrasonography Methods 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 235000019441 ethanol Nutrition 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 17
- 238000006243 chemical reaction Methods 0.000 abstract description 16
- 238000000034 method Methods 0.000 abstract description 15
- 230000015556 catabolic process Effects 0.000 abstract description 14
- 238000006731 degradation reaction Methods 0.000 abstract description 14
- 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 abstract description 10
- 238000003756 stirring Methods 0.000 abstract description 10
- 239000013078 crystal Substances 0.000 abstract description 9
- 238000006555 catalytic reaction Methods 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 6
- 238000004090 dissolution Methods 0.000 abstract description 4
- 239000002243 precursor Substances 0.000 abstract description 4
- 229940106691 bisphenol a Drugs 0.000 abstract description 3
- 239000002904 solvent Substances 0.000 abstract description 3
- 239000000356 contaminant Substances 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 abstract description 2
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 abstract 3
- IOLCXVTUBQKXJR-UHFFFAOYSA-M potassium bromide Chemical compound [K+].[Br-] IOLCXVTUBQKXJR-UHFFFAOYSA-M 0.000 abstract 2
- 239000002086 nanomaterial Substances 0.000 abstract 1
- 238000004065 wastewater treatment Methods 0.000 abstract 1
- CBACFHTXHGHTMH-UHFFFAOYSA-N 2-piperidin-1-ylethyl 2-phenyl-2-piperidin-1-ylacetate;dihydrochloride Chemical compound Cl.Cl.C1CCCCN1C(C=1C=CC=CC=1)C(=O)OCCN1CCCCC1 CBACFHTXHGHTMH-UHFFFAOYSA-N 0.000 description 26
- YFSUTJLHUFNCNZ-UHFFFAOYSA-M 1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,8-heptadecafluorooctane-1-sulfonate Chemical compound [O-]S(=O)(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F YFSUTJLHUFNCNZ-UHFFFAOYSA-M 0.000 description 14
- SNGREZUHAYWORS-UHFFFAOYSA-N perfluorooctanoic acid Chemical group OC(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F SNGREZUHAYWORS-UHFFFAOYSA-N 0.000 description 11
- 229920006926 PFC Polymers 0.000 description 7
- 229910052794 bromium Inorganic materials 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 7
- 230000003197 catalytic effect Effects 0.000 description 6
- 230000002688 persistence Effects 0.000 description 5
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 4
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 4
- 239000002957 persistent organic pollutant Substances 0.000 description 4
- -1 polytetrafluoroethylene Polymers 0.000 description 4
- 229910002651 NO3 Inorganic materials 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000003708 ampul Substances 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 238000009833 condensation Methods 0.000 description 3
- 230000005494 condensation Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000010348 incorporation Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000010453 quartz Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 230000000593 degrading effect Effects 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 2
- 229910052753 mercury Inorganic materials 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 238000002336 sorption--desorption measurement Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 1
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 description 1
- 206010021703 Indifference Diseases 0.000 description 1
- UOZDOLIXBYLRAC-UHFFFAOYSA-L [2-hydroxy-3-(trimethylazaniumyl)propyl]-trimethylazanium;diiodide Chemical compound [I-].[I-].C[N+](C)(C)CC(O)C[N+](C)(C)C UOZDOLIXBYLRAC-UHFFFAOYSA-L 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- QZQVBEXLDFYHSR-UHFFFAOYSA-N gallium(III) oxide Inorganic materials O=[Ga]O[Ga]=O QZQVBEXLDFYHSR-UHFFFAOYSA-N 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 description 1
- 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 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000004811 liquid chromatography Methods 0.000 description 1
- 230000013011 mating Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000005374 membrane filtration Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- BWOROQSFKKODDR-UHFFFAOYSA-N oxobismuth;hydrochloride Chemical compound Cl.[Bi]=O BWOROQSFKKODDR-UHFFFAOYSA-N 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 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
- B01J27/06—Halogens; Compounds thereof
-
- B01J35/39—
-
- B01J35/61—
-
- 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
- C02F1/32—Treatment of water, waste water, or sewage by irradiation with ultraviolet light
-
- 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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/36—Organic compounds containing halogen
-
- 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
- C02F2101/40—Organic compounds containing sulfur
-
- 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 discloses a kind of preparation processes of the excellent novel BiOX solid solution of photocatalysis performance, are related to nano material photocatalysis field.Steps are as follows: by by the ethylene glycol precursor solution of five nitric hydrate bismuths of ultrasonic dissolution, potassium iodide and potassium bromide composition, being placed in reaction kettle and carries out solvent thermal reaction, obtain novel B iOI1-xBrx solid solution.Novel solid solution synthesized by ultrasonic wave added dissolution solvent thermal method provided by the invention is more preferable than conventional solid solution body degradation of contaminant effect synthesized by stirring and dissolving solvent-thermal method.Active crystal face exposure ratio, specific surface area and the light absorpting ability of novel solid solution are apparently higher than BiOI simultaneously, so that photocatalysis performance is more excellent, can efficiently remove the perfluorochemical in water removal under ultraviolet light, bisphenol-A in water removal is efficiently removed under simulated solar irradiation.The application for being light-catalyzed reaction in terms of wastewater treatment provides good material foundation and method of modifying.
Description
Technical field:
The present invention relates to nano-photocatalyst material and environmental applications field, specially a kind of novel BiOX solid solution light
The preparation process of catalysis material and the application study of efficient degradation persistence organic pollutant.
Background technique:
It is current environment dirt using the photocatalysis technology of solar energy degradation of contaminant, especially persistence organic pollutant
Contaminate improvement field there is an urgent need to technology.
Under the background that current water pollution situation is got worse, a kind of persistence organic pollutant --- perfluorochemical
(PFCs) environmental pollution and removal technology is subject to the people's attention.PFCs has due to the C-F bond structure of its high bond energy
The advantages that thermal stability, chemical stability and high surface, be widely used as always in the past few decades surfactant,
In the production of the industrial and agricultural products such as fire retardant.Investigation discovery in recent years, due to being widely applied, PFCs is situated between in a variety of environment
It is detected extensively in matter, wherein detection frequency highest, polluting highest is perfluoro caprylic acid (PFOA) and perfluorooctane sulfonate (PFOS)
Two kinds.A large amount of research discloses PFCs with environmental persistence, biological accumulation effect and extensive bio-toxicity in recent years.PFOS
Deng by Convention of Stockholm tissue positioning persistence organic pollutant.Therefore, it finds efficiently and economic environment disappears
Except PFCs technology becomes one of the hot spot of current environment area research.Wherein, in various processing techniques, photocatalysis technology by
In efficient, environmentally friendly, at low cost the features such as, the application prospect in water process is concerned.This patent trial prepares one kind can be high
Effect degradation PFCs catalysis material and mating degradation technique, for the pollutants such as PFCs environment remove provide effective material and
Technology.
Bismuth oxyiodide (BiOI), due to its special layer structure and good photocatalysis performance, in numerous visible lights
It occupies an important position in catalysis material, there is very good application prospect.But photo-generate electron-hole it is easily multiple and
The drawbacks of, greatly limit its application.Therefore, many researchers attempt to mention by the regulation of different morphologies, composition, structure etc.
The purpose of its high catalytic activity, wherein it is the important of enhancing BiOI performance that solid solution is prepared by introducing two kinds of halogens of Cl, Br
Approach.Since BiOCl, BiOBr and BiOI have similar layer structure and atomic arrangement, Cl, Br are easy to incorporation BiOI's
In lattice, BiOI is formed1-xYxThe solid solution of (Y=Cl, Br).The formation of solid solution causes the crystal structure of BiOI to be finely tuned,
Band gap width changes, and conduction band valence band location changes, and promotes photo-generate electron-hole to efficiently separating, and then be greatly improved
The photocatalysis performance of BiOI.In recent years, there are many material preparation report of solid solution, but for bromine incorporation, it is especially micro
The influence of the incorporation of bromine is studied less.Currently, the preparation of BiOI solid solution, generallys use solvent-thermal method technique, moreover, surrounding
In the critical process step that bismuth source and propiodal disperse in a solvent, dissolves, people are generally confined to conventional stirring technique, still lack
The research of influence of the introducing of other weary aid dispersions, dissolution process for material property.This patent is adulterated using Bromide, is drawn
Enter ultrasonic aid dispersion dissolving technology, trial prepares novel BiOI1-xBrxSolid solution, and answering for the PFOA and PFOS that degrades
With.
Summary of the invention:
The purpose of the present invention is to provide a kind of novel B iOI1-xBrxThe preparation process of solid solution, and have by the material
Effect removal perfluorochemical.The novel B iOI synthesized by the method1-xBrxSolid solution has good drop to perfluorochemical
Effect is solved, to effectively expand the synthetic method of catalysis material, enriches the application of removal hard-degraded substance.
Above-mentioned purpose that the invention is realized by the following technical scheme:
1. a kind of preparation process of the excellent novel BiOX solid solution of photocatalysis performance, the specific steps of which are as follows:
1) by Bi (NO3)3·5H2O is dissolved in ethylene glycol, ultrasonic wiring solution-forming;
2) KI is dissolved in ethylene glycol, ultrasonic wiring solution-forming;
3) 2) solution is added into 1) solution;
4) KBr is added in 3) solution, ultrasound is completely dissolved until KBr;
5) 4) made solution is transferred to autoclave, is placed in baking oven and heats, then cooling, cleaning, drying obtain
BiOI1-xBrx(x=0.05).
2. novel B iOI as described in claim 11-xBrxThe preparation process of solid solution, it is characterised in that: in step 1), Bi
(NO3)3·5H2O is 0.97g, ethylene glycol 20ml, ultrasound 30 minutes.
3. novel B iOI as described in claim 11-xBrxThe preparation process of solid solution, it is characterised in that: in step 2), KI
For 0.32g, ethylene glycol 20ml, ultrasound 30 minutes.
4. novel B iOI as described in claim 11-xBrxThe preparation process of solid solution, it is characterised in that: in step 4),
KBr is 0.01g, ultrasound 10 minutes.
5. novel B iOI as described in claim 11-xBrxThe preparation process of solid solution, it is characterised in that: in step 5), add
Hot temperature is 160 DEG C, keeps 12h, cleans to be cleaned with ethyl alcohol and deionized water, and drying temperature and time are 60 DEG C and 12h.
Novel B iOI provided by the invention1-xBrxThe preparation process of solid-solution material greatly improves the specific surface area of BiOI
And photoelectric properties, and Pair production is efficiently separated, so that the catalytic effect of photochemical catalyst is significantly improved, so that ultraviolet
The perfluorochemical in water removal, the method for enriching materials synthesis can be efficiently gone under light;Process is simple simultaneously, is applicable to big
Batch production.
Detailed description of the invention:
Fig. 1 is BiOI and novel B iOI in embodiment 11-xBrx(x=0.05) X-ray diffraction (XRD) map of solid solution;
Fig. 2 is BiOI and novel B iOI in embodiment 11-xBrx(x=0.05) solid solution scanning electron microscope (SEM)
Figure;
Fig. 3 is BiOI and novel B iOI in embodiment 11-xBrx(x=0.05) solid solution UV-Vis DRS (UV-
Vis) map;
Fig. 4 is the performance schematic diagram of embodiment 2 degrading perfluorinated sad (PFOA);
Fig. 5 is the performance schematic diagram of 3 degrading perfluorinated perfluoroetane sulfonic acid (PFOS) of embodiment;
Fig. 6 is the performance schematic diagram of the degradation of embodiment 4 bisphenol-A (BPA).
Specific embodiment:
The following examples are further illustrations of the invention, rather than limiting the invention.
Embodiment 1: preparation novel B iOI1-xBrx(x=0.05) solid solution
1) by 0.97g Bi (NO3)3·5H2O is dissolved in 20ml ethylene glycol, ultrasonic 30min wiring solution-forming;
2) 0.32g KI is dissolved in another 20ml ethylene glycol, ultrasonic 30min wiring solution-forming;
3) 2) gained liquor kalii iodide is slowly added into 1) gained bismuth nitrate solution, shakes up to obtain yellow transparent molten
Liquid;
4) 0.01g KBr is added to ultrasound in 3) and obtains yellow transparent solution;
5) it by 4) made precursor solution, is transferred in 50ml polytetrafluoroethylene (PTFE) autoclave, sealing is placed in baking oven
160 DEG C of heating 12h, it is cooling;
6) membrane filtration is cleaned with ethyl alcohol and deionized water, dries 12h at 60 DEG C, obtains novel B iOI1-xBrx(x=
0.05) solid solution.
7) composite material of other dopings changes the amount of KI and KBr respectively.
8) ultrasound is changed to stirring and obtains conventional BiOI1-xBrx(x=0.05) solid solution.
Novel B iOI obtained in embodiment 11-xBrx(x=0.05) solid solution determines crystal plane structure and group by XRD
At, by SEM carry out morphology characterization, its optical absorption characteristics is characterized by UV-Vis DRS.As shown in Figure 1, through excessive
Analysis, compared with BiOI, novel B iOI1-xBrx(x=0.05) solid solution and routine BiOI1-xBrx(x=0.05) solid solution is occurred
Characteristic peak it is mobile slightly towards high angle direction, rather than the simple superposition of BiOI and BiOBr illustrates synthesized material not
It is the simple physical mixing of BiOI and BiOBr, but bromine enters in BiOI lattice, forms composite material;As can be seen that novel
BiOI1-xBrx(x=0.05) { 001 } crystal face characteristic peak corresponding with { 002 } crystal face is significantly larger than BiOI and routine in solid solution
BiOI1-xBrx(x=0.05) corresponding peak in solid solution, and the intensity at other peaks is of substantially equal, this is because in ultrasound condition
Under, the addition of bromine changes high preferred orientation, so that { 001 } crystal face and { 002 } crystal face are easier to expose.It is worth noting that, super
Two kinds of dissolution mechanisms of sound and stirring are only for BiOI1-xBrxThe synthesis of solid solution is had any different, for BiOI composite result simultaneously
Indifference.As for novel B iOI1-xBrx(x=0.05) { 001 } crystal face spy corresponding with { 002 } crystal face is only shown in solid solution
Peak is levied, that, so that other peaks seem especially small or even invisible, is actually passed soft because the intensity at the two peaks is too big
The intensity of part analysis, other peaks has no much variations compared to BiOI.As shown in Fig. 2, petal-like structures are presented in BiOI, it is novel
BiOI1-xBrx(x=0.05) flaky nanometer structure is presented in solid solution, and pore structure is obviously more intensive than BiOI, to greatly increase
The specific surface area of material, active site quantity and transmission channel, and then greatly promote light-catalyzed reaction.As shown in figure 3, novel
BiOI1-xBrx(x=0.05) solid solution is about 3 times of BiOI in 600nm optical absorption intensity below, is also had in 600nm or more
It is relatively strong to absorb, and BiOI is almost nil in 600nm or more optical absorption intensity, this is allowed under same illumination condition, novel
BiOI1-xBrx(x=0.05) more light can be absorbed and utilized in solid solution, to greatly speed up light-catalyzed reaction.
Embodiment 2: novel B iOI1-xBrx(x=0.05) perfluoro caprylic acid (PFOA) is removed under solid solution ultraviolet light
Perfluoro caprylic acid (PFOA) aqueous solution for being 20mg/L with deionized water compound concentration takes 30ml that light reaction is added
In quartz ampoule, 12mg novel B iOI is then added1-xBrx(x=0.05) material, and magnetic stir bar is added, it is put into light reaction dress
It sets, opening condensation water management reaction temperature is 25 DEG C, then opens power supply, opens stirring button, first carries out dark reaction and reaches suction
Attached desorption equilibrium, then lamp is turned on, lamp power is 300W mercury lamp, and the concentration of reaction front and back PFOA is by liquid chromatogram measuring, as a result
As shown in figure 4, novel B iOI1-xBrxRemoval rate reaches 99% after solid solution precursor reactant 120 minutes, and BiOI and routine BiOI1- xBrxRemoval rate only reaches 70% and 64% respectively after solid solution precursor reactant 120 minutes, and the β-Ga2O3 of report is in 254nm ultraviolet lighting
Penetrating 3h is only that 38%, TiO2 irradiates 8h degradation rate under ultraviolet light and is also only 35% to the degradation rate of PFOA.Illustrate novel
BiOI1-xBrxSolid solution has extraordinary catalytic degradation performance for PFOA.
Embodiment 3: novel B iOI1-xBrx(x=0.05) perfluorooctane sulfonate (PFOS) is removed under solid solution ultraviolet light
Perfluorooctane sulfonate (PFOS) aqueous solution for being 20mg/L with deionized water compound concentration takes 30ml that light reaction is added
In quartz ampoule, 12mg novel B iOI is then added1-xBrx(x=0.05) material, and magnetic stir bar is added, it is anti-to be put into light
Device is answered, opening condensation water management reaction temperature is 25 DEG C, then opens power supply, opens stirring button, first carries out dark reaction and reaches
It is balanced to adsorption/desorption, then turns on lamp, lamp power is 300W mercury lamp, and the concentration of reaction front and back PFOS is joined by liquid chromatography mass
It is measured with instrument, as a result as shown in figure 5, PFOS removal rate reaches 91% after reaction 120 minutes;It is reported that in P25 catalytic action
Under, removal rate of the PFOS in 300W Hg lamp irradiation 8h is only 19.9%, it is seen that novel B iOI1-xBrx(x=0.05) solid solution pair
There is extraordinary catalytic degradation performance in PFOS.
Embodiment 4: novel B iOI1-xBrx(x=0.05) it is efficiently removed under solid solution simulated solar irradiation bisphenol-A (BPA)
To investigate novel B iOI1-xBrx(x=0.05) degradation effect and simulation of the solid solution to other hard-degraded substances
Degradation efficiency under sunlight chooses representative bisphenol-A (BPA) as object.It is with deionized water compound concentration
Bisphenol-A (BPA) aqueous solution of 10mg/L takes 30ml to be added in the quartz ampoule of light reaction, and 15mg novel B iOI is then added1- xBrx(x=0.05) material, and magnetic stir bar is added, it is put into apparatus for photoreaction, opening condensation water management reaction temperature is 25
DEG C, power supply is then opened, stirring button is opened, dark reaction is first carried out and reaches adsorption/desorption balance, then turn on lamp, lamp power is
800W xenon lamp, the concentration of reaction front and back BPA is by liquid chromatogram measuring, as a result as shown in fig. 6,30 minutes degradation rates reach
100%, and it is reported that the efficiency for the BPA that degrades in BiOI 30 minutes only has 50%, it is seen that novel B iOI1-xBrx(x=0.05) solid
Solution has extraordinary catalytic degradation performance for PFOS.
Claims (5)
1. a kind of preparation process of the excellent novel BiOX solid solution of photocatalysis performance, the specific steps of which are as follows:
1) by Bi (NO3)3·5H2O is dissolved in ethylene glycol, ultrasonic wiring solution-forming;
2) KI is dissolved in ethylene glycol, ultrasonic wiring solution-forming;
3) 2) solution is added into 1) solution;
4) KBr is added in 3) solution, ultrasound is completely dissolved until KBr;
5) 4) made solution is transferred to autoclave, is placed in baking oven and heats, then cooling, cleaning, drying obtain
BiOI1-xBrx(x=0.05).
2. novel B iOI as described in claim 11-xBrxThe preparation process of solid solution, it is characterised in that: in step 1), Bi
(NO3)3·5H2O is 0.97g, ethylene glycol 20ml, ultrasound 30 minutes.
3. novel B iOI as described in claim 11-xBrxThe preparation process of solid solution, it is characterised in that: in step 2), KI is
0.32g, ethylene glycol 20ml, ultrasound 30 minutes.
4. novel B iOI as described in claim 11-xBrxThe preparation process of solid solution, it is characterised in that: in step 4), KBr is
0.01g, ultrasound 10 minutes.
5. novel B iOI as described in claim 11-xBrxThe preparation process of solid solution, it is characterised in that: in step 5), heating temperature
Degree is 160 DEG C, keeps 12h, cleans to be cleaned with ethyl alcohol and deionized water, and drying temperature and time are 60 DEG C and 12h.
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