CN108435216A - A kind of bismuth compound iodine bismuth oxide photocatalyst and preparation method thereof containing iodide ion defect - Google Patents
A kind of bismuth compound iodine bismuth oxide photocatalyst and preparation method thereof containing iodide ion defect Download PDFInfo
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- CN108435216A CN108435216A CN201810341915.7A CN201810341915A CN108435216A CN 108435216 A CN108435216 A CN 108435216A CN 201810341915 A CN201810341915 A CN 201810341915A CN 108435216 A CN108435216 A CN 108435216A
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- bismuth
- iodide ion
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- oxide photocatalyst
- compound iodine
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 132
- 230000007547 defect Effects 0.000 title claims abstract description 117
- XMBWDFGMSWQBCA-UHFFFAOYSA-M iodide Chemical compound [I-] XMBWDFGMSWQBCA-UHFFFAOYSA-M 0.000 title claims abstract description 105
- 229940006461 iodide ion Drugs 0.000 title claims abstract description 105
- -1 bismuth compound iodine bismuth oxide Chemical class 0.000 title claims abstract description 81
- 238000002360 preparation method Methods 0.000 title claims abstract description 47
- 239000003054 catalyst Substances 0.000 claims abstract description 39
- 238000013019 agitation Methods 0.000 claims abstract description 29
- 238000005406 washing Methods 0.000 claims abstract description 23
- 150000001875 compounds Chemical class 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 75
- 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 claims description 70
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 claims description 66
- 239000013049 sediment Substances 0.000 claims description 62
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 claims description 60
- 229910001868 water Inorganic materials 0.000 claims description 55
- 239000002135 nanosheet Substances 0.000 claims description 54
- 229910052797 bismuth Inorganic materials 0.000 claims description 48
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 48
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 30
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims description 26
- 229910052740 iodine Inorganic materials 0.000 claims description 26
- 239000011630 iodine Substances 0.000 claims description 26
- 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 25
- 239000003638 chemical reducing agent Substances 0.000 claims description 20
- 239000008367 deionised water Substances 0.000 claims description 20
- 229910021641 deionized water Inorganic materials 0.000 claims description 20
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 claims description 20
- 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 description 17
- 238000000034 method Methods 0.000 claims description 16
- 235000019441 ethanol Nutrition 0.000 claims description 15
- 239000003795 chemical substances by application Substances 0.000 claims description 13
- 238000007254 oxidation reaction Methods 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 12
- 230000003647 oxidation Effects 0.000 claims description 12
- 239000012279 sodium borohydride Substances 0.000 claims description 11
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 11
- 239000008236 heating water Substances 0.000 claims description 5
- 230000035484 reaction time Effects 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 230000005855 radiation Effects 0.000 claims description 2
- 230000005540 biological transmission Effects 0.000 abstract description 8
- 230000008859 change Effects 0.000 abstract description 6
- 238000001556 precipitation Methods 0.000 abstract description 6
- 230000005284 excitation Effects 0.000 abstract description 5
- 230000009466 transformation Effects 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 206010001497 Agitation Diseases 0.000 abstract 1
- 239000012071 phase Substances 0.000 description 59
- 230000015556 catabolic process Effects 0.000 description 25
- 238000006731 degradation reaction Methods 0.000 description 25
- 239000003643 water by type Substances 0.000 description 14
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 11
- 150000001622 bismuth compounds Chemical class 0.000 description 10
- 238000004458 analytical method Methods 0.000 description 9
- 230000001699 photocatalysis Effects 0.000 description 9
- 238000012360 testing method Methods 0.000 description 9
- 229910000416 bismuth oxide Inorganic materials 0.000 description 8
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 description 8
- 238000007146 photocatalysis Methods 0.000 description 7
- 230000008569 process Effects 0.000 description 7
- 238000012512 characterization method Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 150000002500 ions Chemical class 0.000 description 6
- 238000011001 backwashing Methods 0.000 description 5
- 230000003197 catalytic effect Effects 0.000 description 5
- PRXLCSIMRQFQMX-UHFFFAOYSA-N [O].[I] Chemical compound [O].[I] PRXLCSIMRQFQMX-UHFFFAOYSA-N 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 4
- 230000005012 migration Effects 0.000 description 4
- 238000013508 migration Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 230000007704 transition Effects 0.000 description 4
- 229920002472 Starch Polymers 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 150000003254 radicals Chemical class 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 238000004611 spectroscopical analysis Methods 0.000 description 3
- 235000019698 starch Nutrition 0.000 description 3
- 239000008107 starch Substances 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N argon Substances [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 150000001621 bismuth Chemical class 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 229910052736 halogen Inorganic materials 0.000 description 2
- 150000002367 halogens Chemical class 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000001338 self-assembly Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- 239000010937 tungsten Substances 0.000 description 2
- 238000003775 Density Functional Theory Methods 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- GQPLMRYTRLFLPF-UHFFFAOYSA-N Nitrous Oxide Chemical class [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 description 1
- IOVCWXUNBOPUCH-UHFFFAOYSA-N Nitrous acid Chemical compound ON=O IOVCWXUNBOPUCH-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- OUUQCZGPVNCOIJ-UHFFFAOYSA-M Superoxide Chemical compound [O-][O] OUUQCZGPVNCOIJ-UHFFFAOYSA-M 0.000 description 1
- URVGHPZOLQFKJZ-UHFFFAOYSA-N [Bi]=O.[I] Chemical compound [Bi]=O.[I] URVGHPZOLQFKJZ-UHFFFAOYSA-N 0.000 description 1
- 238000003916 acid precipitation Methods 0.000 description 1
- 239000000809 air pollutant Substances 0.000 description 1
- 231100001243 air pollutant Toxicity 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000002189 fluorescence spectrum Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- DOTMOQHOJINYBL-UHFFFAOYSA-N molecular nitrogen;molecular oxygen Chemical compound N#N.O=O DOTMOQHOJINYBL-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000005424 photoluminescence Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000012855 volatile organic compound Substances 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/92—Chemical or biological purification of waste gases of engine exhaust gases
- B01D53/94—Chemical or biological purification of waste gases of engine exhaust gases by catalytic processes
- B01D53/9404—Removing only nitrogen compounds
- B01D53/9409—Nitrogen oxides
- B01D53/9413—Processes characterised by a specific catalyst
-
- B01J35/39—
-
- 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
- B01J37/02—Impregnation, coating or precipitation
- B01J37/03—Precipitation; Co-precipitation
- B01J37/031—Precipitation
- B01J37/033—Using Hydrolysis
-
- 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
-
- 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
- B01J37/16—Reducing
Abstract
This application discloses a kind of bismuth compound iodine bismuth oxide photocatalyst and preparation method thereof containing iodide ion defect, the bismuth compound iodine bismuth oxide photocatalyst containing iodide ion defect is obtained by preparation processes such as precipitation, centrifuge washing, magnetic agitations.The bismuth compound iodine bismuth oxide photocatalyst containing iodide ion defect prepared by preparation method shown in the application, pass through the structure of iodide ion defect, several defects intermediate level is formd between the valence band and conduction band of photochemical catalyst, change the excitation transmission path of light induced electron, the Transport And Transformation of photogenerated charge is promoted, and then inhibits the compound of photo-generate electron-hole pair.Also visible light-responded range has been widened, the utilization rate of visible light is improved, the bismuth compound iodine bismuth oxide photocatalyst containing iodide ion defect of preparation is finally made to improve the removal rate to NO.In addition, the production economy of the bismuth compound iodine bismuth oxide photocatalyst containing iodide ion defect prepared by preparation method shown in the application is of low cost.
Description
Technical field
This application involves catalyst field more particularly to a kind of compound bismuth oxyiodide photocatalysis of bismuth containing iodide ion defect
Agent and preparation method thereof.
Background technology
With the progress of mankind's science and technology civilization, industry has obtained developing on a large scale, and automobile is also more and more universal, largely
In discharged nitrous oxides to air.Nitrogen oxides as photochemical fog, acid rain, depletion of the ozone layer pollutant, nitrogen oxides
Have become countries in the world atmosphere pollution urgently to be resolved hurrily.It can be seen that the photocatalysis method of optical drive is as a kind of environmental-friendly
Green technology has all shown good application prospect in environmental pollution purification and solar energy conversion aspect.It can be seen that optical drive
Photocatalysis method nitrogen oxides can be made to occur oxidation reaction under photochemical catalyst effect, generate H2O, nitrate, nitrous acid etc.
And reach innoxious, to environment purification.
Bismuth series photocatalyst has good photocatalytic activity, and can effectively degrade nitrogen oxides.Most of bismuth system light
Catalyst can have visible light catalysis activity by excited by visible light.
But the light quantum transfer efficiency of the bismuth series photocatalyst of prior art preparation is relatively low, photoresponse narrow range, the sun
The presence for the problems such as energy (visible light) utilization rate is low hinders the application of photocatalysis technology.The bismuth system photocatalysis of prior art preparation
Agent cannot build a defect intermediate level between valence band and conduction band, can not change light induced electron and swash from valence band to conduction band transitions
Path is sent out, and then the raising of the transport efficiency of light induced electron can not be promoted.
Invention content
This application provides a kind of bismuth compound iodine bismuth oxide photocatalyst and preparation method thereof containing iodide ion defect leads to
It crosses and prepares the bismuth compound iodine bismuth oxide photocatalyst containing iodide ion defect and can be urged in light due to the formation of iodide ion defect
Several defects intermediate level is built between the valence band and conduction band of agent, is changed light induced electron and is excited road from valence band to conduction band transitions
Diameter enhances the purpose of its visible light catalysis activity to reach the light quantum transfer efficiency for improving photochemical catalyst.
First aspect shows that a kind of compound bismuth oxyiodide light of the bismuth containing iodide ion defect is urged according to an embodiment of the present application
The preparation method of agent, which is characterized in that the method includes：
Deionized water is added in two beakers in S101, and five water bismuth nitrates and potassium iodide are added drop-wise to two burnings respectively
In cup, magnetic agitation is carried out to five water bismuth nitrates and potassium iodide at room temperature, respectively obtains five water bismuth nitrate solutions and potassium iodide
Solution；
Liquor kalii iodide is added drop-wise in five water bismuth nitrate solutions by S102 under condition of water bath heating, staticly settle with it is molten
Brick-red sediment is obtained after liquid separation；
The brick-red sediment centrifuge washing is obtained the first sediment by S103；
First sediment is dried S104, obtains the bismuth oxyiodide nanosheet photocatalyst of pure tetragonal phase；
S105 restores it bismuth oxyiodide nanosheet photocatalyst of pure tetragonal phase with reducing agent, magnetic
It staticly settles after power stirring, then reducing agent solution is added drop-wise in bismuth oxyiodide solution, it is heavy to be stood after magnetic agitation at room temperature
It forms sediment, obtains the second sediment；
S106 will dry it after the second sediment centrifuge washing, obtain the bismuth compound iodine containing iodide ion defect
Bismuth oxide photocatalyst.
Selectable, the temperature of the heating water bath is 70-90 DEG C, and the reaction time of the heating water bath is 1-3h.
Selectable, the solution used in the centrifuge washing is ethyl alcohol and deionized water, and the centrifuge washing includes difference
Successively ethyl alcohol, deionized water respectively wash twice.
Selectable, the molar ratio of the five water bismuth nitrate and the potassium iodide is 1:1.
Selectable, the reducing agent is sodium borohydride.
Selectable, the bismuth oxyiodide nanosheet photocatalyst and the molar ratio of the reducing agent of the pure tetragonal phase are
1:1。
The application second aspect shows a kind of bismuth compound iodine bismuth oxide photocatalyst containing iodide ion defect, described to contain
The bismuth compound iodine bismuth oxide photocatalyst of iodide ion defect under conditions of radiation of visible light to the removal rate of NO be 20%~
41%.
By above technical scheme it is found that the embodiment of the present application provides a kind of compound iodine oxidation of the bismuth containing iodide ion defect
Bismuth photochemical catalyst and preparation method thereof, the method includes deionized water is added in two beakers, by five water bismuth nitrates and
Potassium iodide is added drop-wise to respectively in two beakers, is carried out magnetic agitation to five water bismuth nitrates and potassium iodide at room temperature, is respectively obtained
Five water bismuth nitrate solutions and liquor kalii iodide.Under condition of water bath heating, liquor kalii iodide is added drop-wise to five water bismuth nitrate solutions
In, it staticly settles and obtains brick-red sediment after being detached with solution.By the brick-red sediment centrifuge washing, it is heavy to obtain first
Starch；First sediment is dried, the bismuth oxyiodide nanosheet photocatalyst of pure tetragonal phase is obtained.It will be described pure
The bismuth oxyiodide nanosheet photocatalyst of tetragonal phase restores it with reducing agent, is staticly settled after magnetic agitation, then
Reducing agent solution is added drop-wise in bismuth oxyiodide solution, is staticly settled after magnetic agitation at room temperature, the second sediment is obtained.By institute
It is dried after stating the second sediment centrifuge washing, obtains the bismuth compound iodine bismuth oxide photocatalyst containing iodide ion defect.This
The bismuth compound iodine bismuth oxide photocatalyst containing iodide ion defect prepared by the preparation method exemplified is implemented in application, passes through
The structure of iodide ion defect forms several defects intermediate level between the valence band and conduction band of photochemical catalyst, changes light induced electron
Excitation transmission path, promote the Transport And Transformation of photogenerated charge, and then inhibit the compound of photo-generate electron-hole pair.Simultaneously
Also visible light-responded range has been widened, the utilization rate of visible light is improved, has finally made the bismuth containing iodide ion defect of preparation
Compound iodine bismuth oxide photocatalyst improves the removal rate to NO.In addition, prepared by preparation method shown in the embodiment of the present application
The production economy of the bismuth compound iodine bismuth oxide photocatalyst containing iodide ion defect gone out is of low cost.
Description of the drawings
In order to illustrate more clearly of the technical solution of the application, letter will be made to attached drawing needed in the embodiment below
Singly introduce, it should be apparent that, for those of ordinary skills, without having to pay creative labor,
Other drawings may also be obtained based on these drawings.
Fig. 1 is a kind of flow of the preparation method of the bismuth compound iodine bismuth oxide photocatalyst containing iodide ion defect of the application
Figure；
Fig. 2 be the embodiment of the present application 1,2,3,4,5 prepare pure tetragonal phase bismuth oxyiodide nanosheet photocatalyst and
The XRD diagram of bismuth compound iodine bismuth oxide photocatalyst containing iodide ion defect, (XRD is the abbreviation of X-ray diffraction,
That is X-ray diffraction)；
Fig. 3 is the SEM of the bismuth compound iodine bismuth oxide photocatalyst containing iodide ion defect prepared by the embodiment of the present application 2
Figure, (SEM is the abbreviation of scanning electron microscope, i.e. scanning electron microscope)；
Fig. 4 is the SEM figures of the bismuth oxyiodide nanosheet photocatalyst of pure tetragonal phase prepared by the embodiment of the present application 1；
Fig. 5 is the TEM of the bismuth compound iodine bismuth oxide photocatalyst containing iodide ion defect prepared by the embodiment of the present application 2
Figure, (TEM is the abbreviation of transmission electron microscope, i.e. transmission electron microscope)；
Fig. 6 is the HRTEM of the bismuth compound iodine bismuth oxide photocatalyst containing iodide ion defect prepared by the embodiment of the present application 2
Figure, (HRTEM is the abbreviation of high resolution transmission electron microscope, i.e. high-resolution
Transmission electron microscope)；
Fig. 7 is the bismuth oxyiodide nanosheet photocatalyst of pure tetragonal phase prepared by the embodiment of the present application and contains iodide ion
The SURVERY of the XPS of the bismuth compound iodine bismuth oxide photocatalyst of defect schemes, and (XPS figures are X-ray photoelectron
The abbreviation of spectroscop, i.e. X-ray photoelectron spectroscopic analysis)；
Fig. 8 is the bismuth oxyiodide nanosheet photocatalyst of pure tetragonal phase prepared by the embodiment of the present application and contains iodide ion
The bismuth compound iodine bismuth oxide photocatalyst of defect is after argon ion surface sputters 20nm depth, the height of the Bi 4f of respective crystalline phase
Differentiate XPS figures；
Fig. 9 is the bismuth oxyiodide nanosheet photocatalyst of pure tetragonal phase prepared by the embodiment of the present application 1,2 and contains iodine
The surface photovoltage spectrogram of the bismuth compound iodine bismuth oxide photocatalyst of ion defects；
Figure 10 be the embodiment of the present application 1,2,3,4,5 prepare pure tetragonal phase bismuth oxyiodide nanosheet photocatalyst and
The PL of bismuth compound iodine bismuth oxide photocatalyst containing iodide ion defect schemes, and (PL is the abbreviation of Photoluminescence, i.e.,
Fluorescence Spectra)；
Figure 11 be the embodiment of the present application 1,2,3,4,5 prepare pure tetragonal phase bismuth oxyiodide nanosheet photocatalyst and
The UV-Vis DRS figures of bismuth compound iodine bismuth oxide photocatalyst containing iodide ion defect, (UV-Vis DRS are UV-Visible
Diffuse-reflection spectra, i.e. UV-vis DRS)；
Figure 12 be the embodiment of the present application 1,2,3,4,5 prepare pure tetragonal phase bismuth oxyiodide nanosheet photocatalyst and
Bismuth compound iodine bismuth oxide photocatalyst containing iodide ion defect is under visible light conditions to the degradation efficiency comparison chart of NO degradations；
Figure 13 is the bismuth oxyiodide nanosheet photocatalyst of pure tetragonal phase prepared by the embodiment of the present application 1,2 and contains iodine
The bismuth compound iodine bismuth oxide photocatalyst of ion defects detects figure under visible light conditions to the living radical of NO degradations；
Figure 14 is the bismuth oxyiodide nanosheet photocatalyst of pure tetragonal phase prepared by the embodiment of the present application 1,2 and contains iodine
The bismuth compound iodine bismuth oxide photocatalyst of ion defects detects figure under visible light conditions to the living radical of NO degradations；
Figure 15 is the bismuth oxyiodide nanosheet photocatalyst of pure tetragonal phase prepared by the embodiment of the present application 1,2 and contains iodine
The time-resolved fluorescence life diagram of the bismuth compound iodine bismuth oxide photocatalyst of ion defects；
Figure 16 is the bismuth oxyiodide nanosheet photocatalyst of pure tetragonal phase prepared by the embodiment of the present application 1,2 and contains iodine
The DOS of the bismuth compound iodine bismuth oxide photocatalyst of ion defects schemes, (DOS is Density ofstates, the i.e. density of states)；
Figure 17 is the bismuth oxyiodide nanosheet photocatalyst of pure tetragonal phase prepared by the embodiment of the present application 1,2 and contains iodine
The solid phase EPR figures of the bismuth compound iodine bismuth oxide photocatalyst of ion defects；
Figure 18 is the original position of the bismuth compound iodine bismuth oxide photocatalyst containing iodide ion defect prepared by the embodiment of the present application 2
Infrared figure.
Wherein, BiOI is that the bismuth oxyiodide nanometer sheet light of pure tetragonal phase prepared by the preparation method shown in embodiment 1 is urged
Agent；Bi/BiOI-2 is that the compound bismuth oxyiodide light of the bismuth containing iodide ion defect prepared by the preparation method shown in embodiment 2 is urged
Agent；Bi/BiOI-1 is that the compound bismuth oxyiodide light of the bismuth containing iodide ion defect prepared by the preparation method shown in embodiment 3 is urged
Agent；Bi/BiOI-3 is that the compound bismuth oxyiodide light of the bismuth containing iodide ion defect prepared by the preparation method shown in embodiment 4 is urged
Agent；Bi/BiOI-5 is that the compound bismuth oxyiodide light of the bismuth containing iodide ion defect prepared by the preparation method shown in embodiment 5 is urged
Agent.
Specific implementation mode
With reference to the attached drawing in the application, technical solutions in the embodiments of the present application is clearly and completely described,
Obviously, described embodiment is only a part of the embodiment of the application, instead of all the embodiments.Based in the application
Embodiment, every other embodiment obtained by those of ordinary skill in the art without making creative efforts,
It shall fall within the protection scope of the present invention.
Many details are elaborated in the following description in order to fully understand the application, but the application can be with
It is different from the other modes that describe again using other to implement, those skilled in the art can be without prejudice to the application intension
In the case of do similar popularization, therefore the application is not limited by following public specific embodiment.
Fig. 1 is a kind of system of bismuth compound iodine bismuth oxide photocatalyst containing iodide ion defect shown in the embodiment of the present application
The flow chart of Preparation Method, the method includes：
Deionized water is added in two beakers in S101, and five water bismuth nitrates and potassium iodide are added drop-wise to two burnings respectively
In cup, magnetic agitation is carried out to five water bismuth nitrates and potassium iodide at room temperature, respectively obtains five water bismuth nitrate solutions and potassium iodide
Solution；
Liquor kalii iodide is added drop-wise in five water bismuth nitrate solutions by S102 under condition of water bath heating, staticly settle with it is molten
Brick-red sediment is obtained after liquid separation；
The brick-red sediment centrifuge washing is obtained the first sediment by S103；
First sediment is dried S104, obtains the bismuth oxyiodide nanosheet photocatalyst of pure tetragonal phase；
S105 restores it bismuth oxyiodide nanosheet photocatalyst of pure tetragonal phase with reducing agent, magnetic
It staticly settles after power stirring, then reducing agent solution is added drop-wise in bismuth oxyiodide solution, it is heavy to be stood after magnetic agitation at room temperature
It forms sediment, obtains the second sediment；
S106 will dry it after the second sediment centrifuge washing, obtain the bismuth compound iodine containing iodide ion defect
Bismuth oxide photocatalyst.
Selectable, the temperature of the heating water bath is 70-90 DEG C, and the reaction time of the heating water bath is 1-3h.
Selectable, the solution used in the centrifuge washing is ethyl alcohol and deionized water, and the centrifuge washing includes difference
Successively ethyl alcohol, deionized water respectively wash twice.
Selectable, the molar ratio of the five water bismuth nitrate and the potassium iodide is 1:1.
Selectable, the reducing agent is sodium borohydride.
Selectable, the bismuth oxyiodide nanosheet photocatalyst and the molar ratio of the reducing agent of the pure tetragonal phase are
1:1。
By above technical scheme it is found that the embodiment of the present application provides a kind of compound iodine oxidation of the bismuth containing iodide ion defect
Bismuth photochemical catalyst and preparation method thereof, the method includes deionized water is added in two beakers, by five water bismuth nitrates and
Potassium iodide is added drop-wise to respectively in two beakers, is carried out magnetic agitation to five water bismuth nitrates and potassium iodide at room temperature, is respectively obtained
Five water bismuth nitrate solutions and liquor kalii iodide.Under condition of water bath heating, liquor kalii iodide is added drop-wise to five water bismuth nitrate solutions
In, it staticly settles and obtains brick-red sediment after being detached with solution.By the brick-red sediment centrifuge washing, it is heavy to obtain first
Starch；First sediment is dried, the bismuth oxyiodide nanosheet photocatalyst of pure tetragonal phase is obtained.It will be described pure
The bismuth oxyiodide nanosheet photocatalyst of tetragonal phase restores it with reducing agent, is staticly settled after magnetic agitation, then
Reducing agent solution is added drop-wise in bismuth oxyiodide solution, is staticly settled after magnetic agitation at room temperature, the second sediment is obtained.By institute
It is dried after stating the second sediment centrifuge washing, obtains the bismuth compound iodine bismuth oxide photocatalyst containing iodide ion defect.This
The bismuth compound iodine bismuth oxide photocatalyst containing iodide ion defect prepared by the preparation method exemplified is implemented in application, passes through
The structure of iodide ion defect forms several defects intermediate level between the valence band and conduction band of photochemical catalyst, changes light induced electron
Excitation transmission path, promote the Transport And Transformation of photogenerated charge, and then inhibit the compound of photo-generate electron-hole pair.Simultaneously
Also visible light-responded range has been widened, the utilization rate of visible light is improved, has finally made the bismuth containing iodide ion defect of preparation
Compound iodine bismuth oxide photocatalyst improves the removal rate to NO.In addition, prepared by preparation method shown in the embodiment of the present application
The production economy of the bismuth compound iodine bismuth oxide photocatalyst containing iodide ion defect gone out is of low cost.
Experiment is it is found that the compound bismuth oxyiodide of the bismuth containing iodide ion defect prepared by above-mentioned preparation method by analysis
Its catalytic activity of photochemical catalyst is higher than the catalytic activity of corresponding background, and preparation method is simple, is conducive to actual application.
By being carried out to the bismuth compound iodine bismuth oxide photocatalyst containing iodide ion defect prepared by the embodiment of the present application
Characterization, it can be seen that the bismuth compound iodine bismuth oxide photocatalyst containing iodide ion defect has following characteristic：
(1) the compound iodine oxidation of bismuth to the bismuth oxyiodide nanosheet photocatalyst of pure tetragonal phase and containing iodide ion defect
Bismuth photochemical catalyst carries out XRD analysis (as shown in Figure 2), it was demonstrated that has prepared the compound bismuth oxyiodide light of the bismuth containing iodide ion defect
Catalyst.
(2) to the bismuth oxyiodide nanosheet photocatalyst of pure tetragonal phase, the compound iodine oxidation of the bismuth containing iodide ion defect
Bismuth photochemical catalyst carries out sem analysis (as shown in Figure 3,4), it was demonstrated that prepared by the preparation method shown in the embodiment of the present application 2 contains
The bismuth compound iodine bismuth oxide photocatalyst of iodide ion defect stacks self assembly by the nanometer sheet of stratiform and forms；It is lacked to containing iodide ion
Sunken bismuth compound iodine bismuth oxide photocatalyst carries out tem analysis (as shown in Figure 5), can further confirm that the embodiment of the present application is shown
Preparation method prepare the bismuth compound iodine bismuth oxide photocatalyst containing iodide ion defect by the self assembly of laminar nano piece and
At class cavernous body appearance structure.
(3) HRTEM analyses (as shown in Figure 6) are carried out to the bismuth compound iodine bismuth oxide photocatalyst containing iodide ion defect,
Clearly lattice fringe can be observed.
(4) to the bismuth oxyiodide nanosheet photocatalyst of pure tetragonal phase, the compound iodine oxidation of the bismuth containing iodide ion defect
Bismuth photochemical catalyst carries out XPS analysis (as shown in Figure 7), it was demonstrated that in the bismuth compound iodine bismuth oxide photocatalyst containing iodide ion defect
There are Bi, I, O, C elements.
(5) to the bismuth oxyiodide nanosheet photocatalyst containing pure tetragonal phase and the bismuth compound iodine containing iodide ion defect
Bismuth oxide photocatalyst carries out the high-resolution XPS figures of the Bi 4f of its crystalline phase after argon ion surface sputters 20nm depth
It analyzes (as shown in Figure 8), there is the peak position of zeroth order bismuth element to be formed after sputtering can be observed, it was confirmed that there is bismuth simple substance to generate in iodine
On bismuth oxide photocatalyst.
(6) to the bismuth oxyiodide nanosheet photocatalyst of pure tetragonal phase, the compound iodine oxidation of the bismuth containing iodide ion defect
Bismuth photochemical catalyst carries out surface photovoltaic spectroscopy test analysis (as shown in Figure 9), it was demonstrated that the bismuth compound iodine oxygen containing iodide ion defect
Changing bismuth photochemical catalyst makes surface photovoltage intensity increase, and electron mobility increases.
(7) to the bismuth oxyiodide nanosheet photocatalyst of pure tetragonal phase, the compound iodine oxidation of the bismuth containing iodide ion defect
Bismuth photochemical catalyst carries out PL test analysis (as shown in Figure 10), it was demonstrated that the compound bismuth oxyiodide photocatalysis of the bismuth containing iodide ion defect
Agent makes PL strength reductions, promotes the separation in light induced electron and hole.
(8) to the bismuth oxyiodide nanosheet photocatalyst of pure tetragonal phase, the compound iodine oxidation of the bismuth containing iodide ion defect
Bismuth photochemical catalyst carries out UV-Vis DRS analyses (as shown in figure 11), it was demonstrated that the compound bismuth oxyiodide light of the bismuth containing iodide ion defect
Catalyst can increase the absorbability of light in ultraviolet-visible-infrared region, widen light abstraction width, while having occurred red
Move phenomenon.
(9) to the bismuth oxyiodide nanosheet photocatalyst of pure tetragonal phase, the compound iodine oxidation of the bismuth containing iodide ion defect
Bismuth photochemical catalyst agent carries out time-resolved fluorescence life test analysis (as shown in figure 15), it was demonstrated that the bismuth containing iodide ion defect is multiple
The fluorescence lifetime for closing bismuth oxyiodide photochemical catalyst increases, the centrifugation enhancing in light induced electron and hole.
Bismuth compound iodine oxygen of the application to the bismuth oxyiodide nanosheet photocatalyst of pure tetragonal phase, containing iodide ion defect
Change bismuth properties of catalyst to be tested.Test process is as follows：
(1) it is lacked by the bismuth oxyiodide nanosheet photocatalyst of pure tetragonal phase prepared by 0.2 gram of embodiment, containing iodide ion
Sunken bismuth compound iodine bismuth oxide photocatalyst is placed in NO continuous flows in reactor.
(2) under dark condition, when NO concentration reaches balance, it is the halogen tungsten lamp of 150W as visible light to use power
Source, and with the edge filter filtering ultraviolet light of 420nm, when NO concentration reaches balance to the bismuth oxyiodide of pure tetragonal phase
Nanosheet photocatalyst and bismuth compound iodine bismuth oxide photocatalyst containing iodide ion defect are irradiated.
The condition of above-mentioned catalytic performance test process is：Relative humidity 60%, oxygen content 21%, the flow of NO air-flows
Initial concentration for 2.4L/min, NO is 500ppb.
The drop that bismuth compound iodine bismuth oxide photocatalyst provided by the embodiments of the present application containing iodide ion defect degrades to NO
Solution effect is as follows：
(1) the bismuth compound iodine bismuth oxide photocatalyst containing iodide ion defect is that 20%-41% (such as schemes to the degradation rate of NO
Shown in 12), to be apparently higher than degradation rate of the bismuth oxyiodide nanosheet photocatalyst to NO of pure tetragonal phase, the calculating of degradation rate
Formula is that η (%)=(1-C/C0) × 100%, C0 is initial NO concentration, and C is the instantaneous concentration of NO after illumination 30min.
(2) superoxide anion (O2-) and hydroxyl radical free radical (OH) are the compound iodine oxidations of the bismuth containing iodide ion defect
Bismuth photochemical catalyst is degraded the principal degradation free radical of NO under visible light conditions (as shown in Figure 13,14).
(3) compared to the bismuth oxyiodide nanometer sheet photocatalysis of pure tetragonal phase it can be seen from Density function theory
Agent, the bismuth compound iodine bismuth oxide photocatalyst containing iodide ion defect after reducing agent is further processed, iodide ion defect
Defect intermediate level is respectively formd between valence band and conduction band at its.This changes light induced electron and excites road from valence band to conduction band transitions
Diameter becomes the migration pattern of valence band → defect intermediate level → conduction band from original electronics from the migration path of valence band → conduction band.Have
Effect improves the transport efficiency of light induced electron, inhibits the compound of photo-generate electron-hole pair to a certain extent, improves well
Catalyst is under visible light to the degradation rate of NO (as shown in figure 16).
(4) the bismuth oxyiodide nanosheet photocatalyst of the pure tetragonal phase after reducing agent is further processed, compared to
The bismuth oxyiodide nanosheet photocatalyst of its pure tetragonal phase not being further processed, the signal peak enhanced in figure are regarded as
The signal of iodide ion defect.This also illustrates that iodide ion defect is successfully built in bismuth compound iodine bismuth oxide photocatalyst (as schemed
Shown in 17).
(5) compared to the bismuth oxyiodide nanosheet photocatalyst of pure tetragonal phase, the bismuth oxyiodide containing iodide ion defect
In the In-situ Infrared collection of illustrative plates of photochemical catalyst there is intermediate product NO+, it was demonstrated that the conversion road of iodide ion defective effect NO degradations
Diameter, promotes the Transport And Transformation of photo-generated carrier, while being conducive to the absorption and conversion of NO, promotes photochemical catalyst to NO pollutants
Removal performance (as shown in figure 18).
Embodiment 1：
(1) it is added in the 50ml beakers containing 25mL deionized waters and the 25ml beakers containing 10ml deionized waters respectively
The molar ratio of five water bismuth nitrates and potassium iodide, the two addition is 1:1, magnetic agitation 30 minutes, respectively obtain five at room temperature
Water bismuth nitrate solution and liquor kalii iodide；
Liquor kalii iodide is added drop-wise in five water bismuth nitrate solutions under (2) 80 DEG C of condition of water bath heating, reacts 2h, it is heavy to stand
It forms sediment and the isolated brick-red sediment of solution；
(3) by the brick-red sediment ethyl alcohol and deionized water, front and back washing is each twice respectively, obtains the first precipitation
Object；
(4) first sediment is dried under the conditions of 60 DEG C in an oven, obtains the iodine oxygen of pure tetragonal phase
Change bismuth nanosheet photocatalyst.
To the embodiment of the present application prepare pure tetragonal phase bismuth oxyiodide nanosheet photocatalyst by XRD, SEM,
TEM, HRTEM, XPS, surface photovoltaic spectroscopy, PL, UV-Vi s DRS, ESR, EPR, the time-resolved fluorescence service life, In-situ Infrared into
Row characterization.
The bismuth oxyiodide nanosheet photocatalyst of pure tetragonal phase prepared by the embodiment of the present application degrades with true to NO
Its fixed photocatalytic activity, detailed process are：It is 2.4L/ in the flow of relative humidity 60%, oxygen content 21%, NO air-flows
Under conditions of the initial concentration of min, NO are 500ppb, the bismuth oxyiodide containing pure tetragonal phase prepared by 0.2g embodiments is received
It is the halogen tungsten lamp of 150W as visible light source that rice piece photochemical catalyst, which is placed in NO continuous flows and in reactor, uses power, and is used
The edge filter filtering ultraviolet light of 420nm, when NO concentration reaches balance to the bismuth oxyiodide nanometer of the pure tetragonal phase
Piece photochemical catalyst is irradiated, and the pure tetragonal phase bismuth oxyiodide photochemical catalyst of the embodiment of the present application preparation is calculated to NO's
Degradation rate is 2%.
Embodiment 2：
(1) it is added in the 50ml beakers containing 25mL deionized waters and the 25ml beakers containing 10ml deionized waters respectively
The molar ratio of five water bismuth nitrates and potassium iodide, the two addition is 1:1, magnetic agitation 30 minutes, respectively obtain five at room temperature
Water bismuth nitrate solution and liquor kalii iodide；
Liquor kalii iodide is added drop-wise in five water bismuth nitrate solutions under (2) 80 DEG C of condition of water bath heating, reacts 2h, it is heavy to stand
It forms sediment and the isolated brick-red sediment of solution；
(3) by the brick-red sediment ethyl alcohol and deionized water, front and back washing is each twice respectively, obtains the first precipitation
Object；
(4) first sediment is dried under the conditions of 60 DEG C in an oven, obtains the iodine oxygen of pure tetragonal phase
Change bismuth nanosheet photocatalyst；
(5) the bismuth oxyiodide nanosheet photocatalyst and 0.076 gram of sodium borohydride difference of 0.70 gram of pure tetragonal phase are weighed
It is added in the 50ml beakers equipped with 20ml deionized waters, magnetic agitation 20min at room temperature is distinguished, then by sodium borohydride solution
It is added drop-wise in bismuth oxyiodide solution, is staticly settled after magnetic agitation 20min at room temperature, obtain the second sediment；
(6) the second sediment is used again ethyl alcohol and deionized water respectively front and back centrifuge washing respectively twice after, in baking oven 50
It is dried under the conditions of DEG C, finally obtains the bismuth compound iodine bismuth oxide photocatalyst containing iodide ion defect.
The characterization of the bismuth compound iodine bismuth oxide photocatalyst containing iodide ion defect that prepared to the embodiment of the present application and right
The degradation test process of NO is the same as embodiment 1.The bismuth compound iodine containing iodide ion defect of the embodiment of the present application preparation is calculated
Bismuth oxide photocatalyst is 41% to the degradation rate of NO.
Embodiment 3：
(1) it is added in the 50ml beakers containing 25mL deionized waters and the 25ml beakers containing 10ml deionized waters respectively
The molar ratio of five water bismuth nitrates and potassium iodide, the two addition is 1:1, magnetic agitation 30 minutes, respectively obtain five at room temperature
Water bismuth nitrate solution and liquor kalii iodide；
Liquor kalii iodide is added drop-wise in five water bismuth nitrate solutions under (2) 80 DEG C of condition of water bath heating, reacts 2h, it is heavy to stand
It forms sediment and the isolated brick-red sediment of solution；
(3) by the brick-red sediment ethyl alcohol and deionized water, front and back washing is each twice respectively, obtains the first precipitation
Object；
(4) the first sediment is dried under the conditions of 60 DEG C in an oven, obtains the bismuth oxyiodide of pure tetragonal phase
Nanosheet photocatalyst；
(5) the bismuth oxyiodide nanosheet photocatalyst and 0.038 gram of sodium borohydride difference of 0.70 gram of pure tetragonal phase are weighed
It is added in the 50ml beakers equipped with 20ml deionized waters, magnetic agitation 20min at room temperature is distinguished, then by sodium borohydride solution
It is added drop-wise in bismuth oxyiodide solution, is staticly settled after magnetic agitation 20min at room temperature, obtain the second sediment；
(6) the second sediment is used again ethyl alcohol and deionized water respectively front and back centrifuge washing respectively twice after, in baking oven 50
It is dried under the conditions of DEG C, finally obtains the bismuth compound iodine bismuth oxide photocatalyst containing iodide ion defect.
The characterization of the bismuth compound iodine bismuth oxide photocatalyst containing iodide ion defect that prepared to the embodiment of the present application and right
The degradation test process of NO is the same as embodiment 1.The bismuth compound iodine containing iodide ion defect of the embodiment of the present application preparation is calculated
Bismuth oxide photocatalyst is 20% to the degradation rate of NO.
Embodiment 4：
(1) it is added in the 50ml beakers containing 25mL deionized waters and the 25ml beakers containing 10ml deionized waters respectively
The molar ratio of five water bismuth nitrates and potassium iodide, the two addition is 1:1, magnetic agitation 30 minutes, respectively obtain five at room temperature
Water bismuth nitrate solution and liquor kalii iodide；
Liquor kalii iodide is added drop-wise in five water bismuth nitrate solutions under (2) 80 DEG C of condition of water bath heating, reacts 2h, it is heavy to stand
It forms sediment and the isolated brick-red sediment of solution；
(3) by the brick-red sediment ethyl alcohol and deionized water, front and back washing is each twice respectively, obtains the first precipitation
Object；
(4) the first sediment is dried under the conditions of 60 DEG C in an oven, obtains the bismuth oxyiodide of pure tetragonal phase
Nanosheet photocatalyst；
(5) the bismuth oxyiodide nanosheet photocatalyst and 0.113 gram of sodium borohydride difference of 0.70 gram of pure tetragonal phase are weighed
The 50ml beakers equipped with 20ml deionized waters are added in, distinguish magnetic agitation 20min at room temperature, it is then that sodium borohydride is molten
Drop is added in bismuth oxyiodide solution, is staticly settled after magnetic agitation 20min at room temperature, is obtained the second sediment；
(6) the second sediment is used again ethyl alcohol and deionized water respectively front and back centrifuge washing respectively twice after, in baking oven 50
It is dried under the conditions of DEG C, finally obtains the bismuth compound iodine bismuth oxide photocatalyst containing iodide ion defect.
The characterization of the bismuth compound iodine bismuth oxide photocatalyst containing iodide ion defect that prepared to the embodiment of the present application 4 and right
The degradation test process of NO is the same as embodiment 1.The bismuth compound iodine containing iodide ion defect of the embodiment of the present application preparation is calculated
Bismuth oxide photocatalyst is 32% to the degradation rate of NO.
Embodiment 5：
(1) it is added in the 50ml beakers containing 25mL deionized waters and the 25ml beakers containing 10ml deionized waters respectively
The molar ratio of five water bismuth nitrates and potassium iodide, the two addition is 1:1, magnetic agitation 30 minutes, respectively obtain five at room temperature
Water bismuth nitrate solution and liquor kalii iodide；
Liquor kalii iodide is added drop-wise in bismuth nitrate solution under (2) 80 DEG C of condition of water bath heating, react 2h, staticly settle with
The isolated brick-red sediment of solution；
(3) by the brick-red sediment ethyl alcohol and deionized water, front and back washing is each twice respectively, obtains the first precipitation
Object；
(4) the first sediment is dried under the conditions of 60 DEG C in an oven, obtains the bismuth oxyiodide of pure tetragonal phase
Nanosheet photocatalyst；
(5) the bismuth oxyiodide nanosheet photocatalyst and 0.189 gram of sodium borohydride difference of 0.70 gram of pure tetragonal phase are weighed
The 50ml beakers equipped with 20ml deionized waters are added in, distinguish magnetic agitation 20min at room temperature, it is then that sodium borohydride is molten
Drop is added in bismuth oxyiodide solution, is staticly settled after magnetic agitation 20min at room temperature, is obtained the second sediment；
(6) the second sediment is used again ethyl alcohol and deionized water respectively front and back centrifuge washing respectively twice after, in baking oven 50
It is dried under the conditions of DEG C, finally obtains the bismuth compound iodine bismuth oxide photocatalyst containing iodide ion defect.
The characterization of the bismuth compound iodine bismuth oxide photocatalyst containing iodide ion defect that prepared to the embodiment of the present application and right
The degradation test process of NO is the same as embodiment 1.The bismuth compound iodine containing iodide ion defect of the embodiment of the present application preparation is calculated
Bismuth oxide photocatalyst is 26% to the degradation rate of NO.
Table 1 is the degradation rate that each photochemical catalyst degrades to NO in above-described embodiment 1-5：
Table 1 is as can be seen that the bismuth containing iodide ion defect prepared by building iodide ion defect on photochemical catalyst
Compound iodine bismuth oxide photocatalyst to the degradation of NO relative to pure tetragonal phase bismuth oxyiodide nanosheet photocatalyst to NO's
For degradation, the former degradation effect significantly improves.This is because iodide ion defect is formed between photochemical catalyst valence band and conduction band
Several defects intermediate levels, this also just changes light induced electron from valence band to conduction band transitions excitation path, by original electronics from
The migration path of valence band → conduction band becomes the migration pattern of valence band → defect intermediate level → conduction band.Effectively increase light induced electron
Transport efficiency, inhibit the compound of photo-generate electron-hole pair to a certain extent, improve catalyst well under visible light
To the degradation rate of NO.Method economic cost provided by the present application is cheap, and operation is simple.It is generated simultaneously in light using bismuth simple substance
The visible absorption range that photochemical catalyst is improved on catalyst, enhances the performance of photochemical catalyst.
It should be noted that the bismuth compound iodine bismuth oxide photocatalyst provided by the embodiments of the present application containing iodide ion defect
To sulfide, volatile organic compounds, non-NO other air pollutants such as oxynitrides catalytic mechanism with to nitrogen oxygen
The catalytic mechanism of compound is identical, therefore representative by testing the degradation of NO in the embodiment of the present application.
It is apparent to those skilled in the art although describing the application in a manner of specific embodiment
, in the case where not departing from spirit and scope defined by the appended claims, can to the application into
Row variations and modifications, these change and modification are also included in scope of the present application.
By above technical scheme it is found that the embodiment of the present application provides a kind of compound iodine oxidation of the bismuth containing iodide ion defect
Bismuth photochemical catalyst and preparation method thereof, the method includes deionized water is added in two beakers, by five water bismuth nitrates and
Potassium iodide is added drop-wise to respectively in two beakers, is carried out magnetic agitation to five water bismuth nitrates and potassium iodide at room temperature, is respectively obtained
Five water bismuth nitrate solutions and liquor kalii iodide；Under condition of water bath heating, liquor kalii iodide is added drop-wise to five water bismuth nitrate solutions
In, it staticly settles and obtains brick-red sediment after being detached with solution；By the brick-red sediment centrifuge washing, it is heavy to obtain first
Starch；First sediment is dried, the bismuth oxyiodide nanosheet photocatalyst of pure tetragonal phase is obtained；It will be described pure
The bismuth oxyiodide nanosheet photocatalyst of tetragonal phase restores it with reducing agent, is staticly settled after magnetic agitation, then
Reducing agent solution is added drop-wise in bismuth oxyiodide solution, is staticly settled after magnetic agitation at room temperature, the second sediment is obtained；By institute
It is dried after stating the second sediment centrifuge washing, obtains the bismuth compound iodine bismuth oxide photocatalyst containing iodide ion defect.This
The bismuth compound iodine bismuth oxide photocatalyst containing iodide ion defect prepared by the preparation method exemplified is implemented in application, passes through
The structure of iodide ion defect forms several defects intermediate level between the valence band and conduction band of photochemical catalyst, changes light induced electron
Excitation transmission path, promote the Transport And Transformation of photogenerated charge, and then inhibit the compound of photo-generate electron-hole pair.Simultaneously
Also visible light-responded range has been widened, the utilization rate of visible light is improved, has finally made the bismuth containing iodide ion defect of preparation
Compound iodine bismuth oxide photocatalyst improves the removal rate to NO.In addition, prepared by preparation method shown in the embodiment of the present application
The production economy of the bismuth compound iodine bismuth oxide photocatalyst containing iodide ion defect gone out is of low cost.
It the above is only the specific implementation mode of the application, it is noted that those skilled in the art are come
It says, under the premise of not departing from the application principle, several improvements and modifications can also be made, these improvements and modifications also should be regarded as
The protection domain of the application.
Claims (7)
1. a kind of preparation method of the bismuth compound iodine bismuth oxide photocatalyst containing iodide ion defect, which is characterized in that the side
Method includes：
Deionized water is added in two beakers in S101, and five water bismuth nitrates and potassium iodide are added drop-wise to respectively in two beakers,
Magnetic agitation is carried out to five water bismuth nitrates and potassium iodide at room temperature, respectively obtains five water bismuth nitrate solutions and liquor kalii iodide；
Liquor kalii iodide is added drop-wise in five water bismuth nitrate solutions by S102 under condition of water bath heating, is staticly settled and solution point
Brick-red sediment is obtained from after；
The brick-red sediment centrifuge washing is obtained the first sediment by S103；
First sediment is dried S104, obtains the bismuth oxyiodide nanosheet photocatalyst of pure tetragonal phase；
S105 restores it bismuth oxyiodide nanosheet photocatalyst of pure tetragonal phase with reducing agent, and magnetic force stirs
It staticly settles after mixing, then reducing agent solution is added drop-wise in bismuth oxyiodide solution, staticly settle, obtain after magnetic agitation at room temperature
To the second sediment；
S106 will dry it after the second sediment centrifuge washing, obtain the compound iodine oxidation of the bismuth containing iodide ion defect
Bismuth photochemical catalyst.
2. preparation method as described in claim 1, which is characterized in that the temperature of the heating water bath is 70-90 DEG C, the water
The reaction time of bath heating is 1-3h.
3. preparation method as described in claim 1, which is characterized in that solution used in the centrifuge washing be ethyl alcohol and go from
Sub- water, the centrifuge washing include being taken up in order of priority respectively to be washed twice with ethyl alcohol, deionized water.
4. preparation method as described in claim 1, which is characterized in that the molar ratio of the five water bismuth nitrate and the potassium iodide
It is 1:1.
5. preparation method as described in claim 1, which is characterized in that the reducing agent is sodium borohydride.
6. preparation method as described in claim 1, which is characterized in that the bismuth oxyiodide nanometer sheet light of the pure tetragonal phase is urged
Agent and the molar ratio of the reducing agent are 1:1.
7. a kind of bismuth compound iodine bismuth oxide photocatalyst containing iodide ion defect, which is characterized in that described to be lacked containing iodide ion
Sunken bismuth compound iodine bismuth oxide photocatalyst is prepared by the preparation method described in claim 1-6 any one；
The bismuth compound iodine bismuth oxide photocatalyst containing iodide ion defect is under conditions of radiation of visible light to the removal of NO
Rate is 20%~41%.
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| CN111558385A (en) * | 2020-05-13 | 2020-08-21 | 重庆工商大学 | P-n type heterojunction BiOBr/SnO2Composite photocatalyst and preparation method thereof |
| CN113042072A (en) * | 2021-03-15 | 2021-06-29 | 西安科技大学 | Bismuth oxide/defect bismuth oxyiodide composite material, preparation method and application thereof |
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| CN115178280A (en) * | 2022-08-18 | 2022-10-14 | 贵州医科大学 | Bismuth-containing nano antibacterial agent with surface oxygen vacancies and preparation method thereof |
| CN115364873A (en) * | 2022-08-22 | 2022-11-22 | 电子科技大学长三角研究院(湖州) | Hollow tubular ultrathin photocatalyst and preparation method thereof |
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