CN106563411A - Preparation method for snowflake-shaped ZnO/BiOI composite material - Google Patents
Preparation method for snowflake-shaped ZnO/BiOI composite material Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000002131 composite material Substances 0.000 title abstract description 13
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 35
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 30
- 239000002073 nanorod Substances 0.000 claims abstract description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 20
- 239000008367 deionised water Substances 0.000 claims abstract description 20
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 7
- 230000035484 reaction time Effects 0.000 claims abstract description 7
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims description 17
- 239000002904 solvent Substances 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 5
- 238000005516 engineering process Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 230000005855 radiation Effects 0.000 claims description 3
- 239000012046 mixed solvent Substances 0.000 claims description 2
- 239000013049 sediment Substances 0.000 claims description 2
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims 1
- 239000002244 precipitate Substances 0.000 claims 1
- 239000000243 solution Substances 0.000 abstract description 10
- 230000001699 photocatalysis Effects 0.000 abstract description 9
- 239000011259 mixed solution Substances 0.000 abstract description 7
- 238000003760 magnetic stirring Methods 0.000 abstract 2
- 238000004729 solvothermal method Methods 0.000 abstract 2
- 238000001132 ultrasonic dispersion Methods 0.000 abstract 1
- 235000019441 ethanol Nutrition 0.000 description 16
- 125000005909 ethyl alcohol group Chemical group 0.000 description 15
- 238000013019 agitation Methods 0.000 description 11
- 239000003643 water by type Substances 0.000 description 10
- 150000001875 compounds Chemical class 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 5
- 238000000151 deposition Methods 0.000 description 5
- 230000008021 deposition Effects 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 238000007146 photocatalysis Methods 0.000 description 5
- 229910052708 sodium Inorganic materials 0.000 description 5
- 239000011734 sodium Substances 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 4
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- MOTZDAYCYVMXPC-UHFFFAOYSA-N dodecyl hydrogen sulfate Chemical class CCCCCCCCCCCCOS(O)(=O)=O MOTZDAYCYVMXPC-UHFFFAOYSA-N 0.000 description 3
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 3
- 230000004044 response Effects 0.000 description 3
- RZYKUPXRYIOEME-UHFFFAOYSA-N CCCCCCCCCCCC[S] Chemical compound CCCCCCCCCCCC[S] RZYKUPXRYIOEME-UHFFFAOYSA-N 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 2
- 229910052797 bismuth Inorganic materials 0.000 description 2
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 239000002121 nanofiber Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241000372132 Hydrometridae Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- 238000005406 washing 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
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- 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
- B01J27/138—Halogens; Compounds thereof with alkaline earth metals, magnesium, beryllium, zinc, cadmium or mercury
-
- 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/027—Compounds of F, Cl, Br, I
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28033—Membrane, sheet, cloth, pad, lamellar or mat
- B01J20/2804—Sheets with a specific shape, e.g. corrugated, folded, pleated, helical
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- B01J35/39—
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- 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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- 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
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- 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
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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- 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 preparation method for a snowflake-shaped ZnO/BiOI composite material. Firstly, Zn(NO3)3.6H2O and NaOH are dissolved in deionized water; then, lauryl sodium sulfate is dispersed into a mixed solution of absolute ethyl alcohol and deionized water; and next, the two solutions are mixed, and after magnetic stirring is carried out, a microwave-assisted hydrothermal method is adopted, and the flower-shaped ZnO nanorods are obtained. KI and Bi(NO3)3.5H2O are added into ethylene glycol, after a period of magnetic stirring, the prepared flower-shaped ZnO nanorods are added, ultrasonic dispersion is added, and after a solvothermal reaction, the flaxen snowflake-shaped ZnO/BiOI composite material is obtained. Compared with other shapes, the snowflake-shaped ZnO/BiOI composite material is a tightly-stacked laminar BiOI sphere formed on the surfaces of the ZnO nanorods, and the photocatalytic activity is remarkably improved. By means of the solvothermal method, the reaction time and the reaction temperature are controlled easily, equipment is simple, and the cost is low.
Description
Technical field
The present invention relates to a kind of preparation method of flakes ZnO/BiOI composites.
Background technology
The bismuth oxyhalide (BiOX, X-F, Cl, Br, I) of layer structure as the new semiconductor light-catalyst of a class, with
Its good Uv and visible light optical Response and receive much concern.BiOI is used as the one kind in bismuth oxyhalide, and its band gap is narrow
(1.77-1.92eV), preferably absorption characteristic is shown in visible-range, possesses excellent photocatalysis under visible light illumination
Degradation property, but the photo-generate electron-hole of pure BiOI is easily combined, and semiconductors coupling rule can effectively suppress light
The recombination rate of raw carrier, so as to improve the separation rate of carrier, beneficial to the photocatalysis performance for improving material.
(Wang S, Guan Y, the Wang L.Applied Catalysis B such as Wang:Environmental,2015,
168:448-457.) with ethylene glycol as solvent, BiOI/Ag is prepared for through chemical precipitation process using solvent-thermal method3VO4It is compound
Material, under contrast, the visible light photocatalysis active of the compound is much better than single Ag, Ag3VO4And BiOI.Liao etc.
(Liao C,Ma Z,Dong G.Applied Surface Science,2014,314:481-489.) repaiied with BiOI nanometer sheets
Decorations TiO2Nanofiber prepares composite, and cutting is carried out the modification between two kinds of materials by controlling Bi source concentration, and BiOI exists
TiO2Nanofiber surface is uniformly distributed, with very high visible light catalysis activity.(Dai K, the Lu L, Liang such as Dai
C.Dalton Transactions,2015,44:7903-7910.) in the mixed solution of ethanol and deionized water, using water
Hot method is prepared for coaxial C3N4/ BiOI/graphene oxide heterogeneous material compounds, the compound of three effectively inhibits photoproduction
Electron-hole it is compound, so as to improve the catalytic performance of material.
At present, there is not yet the report of the preparation method with regard to flakes ZnO/BiOI composites.
The content of the invention
It is an object of the invention to provide a kind of preparation method of flakes ZnO/BiOI composites.
To achieve these goals, present invention employs technical scheme below：
1) by Zn (NO3)3·6H2O and NaOH are dissolved in deionized water, obtain mixed liquor A, and lauryl sodium sulfate is disperseed
In the mixed solvent of absolute ethyl alcohol and deionized water, mixed liquid B is obtained, 30～40min will be stirred after mixed liquor A and B mixing, so
After carry out microwave assisted aqueous extraction thermal response, by the sediment that obtains of reaction is scrubbed and drying, obtain flower-shaped ZnO nanorod；
2) by KI and Bi (NO3)3·5H2O is stirred to being uniformly dispersed after adding in ethylene glycol, mixed liquor C is obtained, to mixed liquor C
It is middle to add ultrasonic disperse after the flower-shaped ZnO nanorod that obtains of step 1, then carry out solvent thermal reaction, after reaction Jing washings and
Drying, obtains flakes ZnO/BiOI composites.
In the mixed liquor A, Zn (NO3)3·6H2The consumption of O is 0.1～0.9g, and the consumption of NaOH is 0.3～2.5g, is gone
The consumption of ionized water is 1～5mL；In the mixed liquid B, the consumption of lauryl sodium sulfate is 0.1～3g, the use of deionized water
Measure as 10～300mL, the consumption of absolute ethyl alcohol is 1～50mL.
The reaction temperature of the microwave radiation technology hydro-thermal reaction is 100～180 DEG C, and the reaction time is 30～60min.
In the mixed liquor C, the consumption of KI is 0.08～0.2g, Bi (NO3)3·5H2The consumption of O be 0.3～0.6g, second
The consumption of glycol is 10～40mL；The addition of flower-shaped ZnO nanorod is 0.05～0.3g in the mixed liquor C.
In the step 2, mixing time is 35～60min.
In the step 2, the ultrasonic disperse time is 15～30min.
The reaction temperature of the solvent thermal reaction is 110～160 DEG C, and the reaction time is 1h～3h.
In the step 1, the temperature of drying is 60～70 DEG C；In the step 2, the temperature of drying is 80～90 DEG C.
Compared with prior art, the present invention has the advantages that：
The present invention on the basis of ZnO nanorod is prepared, with Bi (NO3)3·5H2O and KI is raw material, in ethylene glycol
In solvent, flakes ZnO/BiOI composites are prepared for using solvent-thermal method, process is simple, reaction temperature and the reaction time it is easy
Control, it is with low cost.Flakes ZnO/BiOI compounds are to prepare spherical BiOI on ZnO nanorod surface, and the composite is big
Specific surface area, can both improve adsorptivity, it is also possible to promote its visible light photocatalysis active, and for preparing high catalytic activity
BiOI also have very big prospect.
Description of the drawings
Fig. 1 is the SEM stereoscan photographs of flower-shaped ZnO nanorod；In FIG, scale is 4 μm.
Fig. 2 is the stereoscan photograph of flakes ZnO/BiOI compounds；In fig. 2, scale is 2 μm.
Fig. 3 is the photocatalytic degradation capability curve of ZnO, BiOI and ZnO/BiOI (prepared by embodiment 4) photochemical catalyst.
Specific embodiment
The present invention is described in further details with reference to the accompanying drawings and examples.The embodiment is the solution to the present invention
Release, rather than limit.
Embodiment 1：
1) by 0.5g Zn (NO3)3·6H2O and 1.5g NaOH are dissolved in 3mL deionized waters, then by 1g dodecyl sulphates
Sodium (SDS) is scattered in the mixed solution of 100mL deionized waters and 25mL absolute ethyl alcohols, then mixes both the above solution,
After magnetic agitation 30min, polytetrafluoroethyltank tank, in being positioned over the microwave dissolver of MDS-10 models, 180 DEG C of hydro-thermal reactions are moved into
White depositions are obtained after 40min, Jing absolute ethyl alcohols and deionized water alternating centrifugal are cleaned 3 times, filtered, and drying is spent
Shape ZnO nanorod.
2) by 0.2g KI and 0.6g Bi (NO3)3·5H2O is added in 40mL ethylene glycol, and magnetic agitation 40min is added
0.2g is by step 1) the flower-shaped ZnO nanorod that obtains, ultrasonic disperse 20min, in pouring autoclave into, 160 DEG C of solvent heats are anti-
3h, Jing absolute ethyl alcohols and deionized water alternating centrifugal is answered to clean 3 times, filter, drying obtains flaxen flakes ZnO/
BiOI composites.
Embodiment 2：
1) by 0.7g Zn (NO3)3·6H2O and 2.5g NaOH are dissolved in 4mL deionized waters, then by 1.7g dodecyl sulphur
Sour sodium (SDS) is scattered in the mixed solution of 100mL deionized waters and 30mL absolute ethyl alcohols, then mixes both the above solution
Close, after magnetic agitation 30min, move into polytetrafluoroethyltank tank, in being positioned over the microwave dissolver of MDS-10 models, 170 DEG C of hydro-thermals
White depositions are obtained after reaction 35min, Jing absolute ethyl alcohols and deionized water alternating centrifugal are cleaned 3 times, filtered, and drying is obtained final product
To flower-shaped ZnO nanorod.
2) by 0.1g KI and 0.38g Bi (NO3)3·5H2O is added in 30mL ethylene glycol, and magnetic agitation 50min is added
0.2g is by step 1) the flower-shaped ZnO nanorod that obtains, ultrasonic disperse 15min, in pouring autoclave into, 130 DEG C of solvent heats are anti-
2h, Jing absolute ethyl alcohols and deionized water alternating centrifugal is answered to clean 3 times, filter, drying obtains flaxen flakes ZnO/
BiOI composites.
Embodiment 3：
1) by 0.3g Zn (NO3)3·6H2O and 1.0g NaOH are dissolved in 5mL deionized waters, then by 2g dodecyl sulphates
Sodium (SDS) is scattered in the mixed solution of 150mL deionized waters and 30mL absolute ethyl alcohols, then mixes both the above solution,
After magnetic agitation 30min, polytetrafluoroethyltank tank, in being positioned over the microwave dissolver of MDS-10 models, 150 DEG C of hydro-thermal reactions are moved into
White depositions are obtained after 35min, Jing absolute ethyl alcohols and deionized water alternating centrifugal are cleaned 3 times, filtered, and drying is spent
Shape ZnO nanorod.
2) by 0.15g KI and 0.5g Bi (NO3)3·5H2O is added in 20mL ethylene glycol, and magnetic agitation 40min is added
0.25g is by step 1) the flower-shaped ZnO nanorod that obtains, ultrasonic disperse 25min, in pouring autoclave into, 150 DEG C of solvent heats are anti-
3h, Jing absolute ethyl alcohols and deionized water alternating centrifugal is answered to clean 3 times, filter, drying obtains flaxen flakes ZnO/
BiOI composites.
Embodiment 4：
1) by 0.2g Zn (NO3)3·6H2O and 0.8g NaOH are dissolved in 3mL deionized waters, then by 0.9g dodecyl sulphur
Sour sodium (SDS) is scattered in the mixed solution of 280mL deionized waters and 30mL absolute ethyl alcohols, then mixes both the above solution
Close, after magnetic agitation 30min, move into polytetrafluoroethyltank tank, in being positioned over the microwave dissolver of MDS-10 models, 150 DEG C of hydro-thermals
White depositions are obtained after reaction 35min, Jing absolute ethyl alcohols and deionized water alternating centrifugal are cleaned 3 times, filtered, and drying is obtained final product
To flower-shaped ZnO nanorod.
2) by 0.08g KI and 0.43g Bi (NO3)3·5H2O is added in 30mL ethylene glycol, magnetic agitation 35min, then is added
Enter 0.28g by step 1) the flower-shaped ZnO nanorod that obtains, ultrasonic disperse 30min, in pouring autoclave into, 120 DEG C of solvent heats
Reaction 2h, Jing absolute ethyl alcohols and deionized water alternating centrifugal are cleaned 3 times, are filtered, and drying obtains flaxen flakes ZnO/
BiOI composites.
Embodiment 5：
1) by 0.6g Zn (NO3)3·6H2O and 1.2g NaOH are dissolved in 2mL deionized waters, then by 2g dodecyl sulphates
Sodium (SDS) is scattered in the mixed solution of 180mL deionized waters and 40mL absolute ethyl alcohols, then mixes both the above solution,
After magnetic agitation 30min, polytetrafluoroethyltank tank, in being positioned over the microwave dissolver of MDS-10 models, 160 DEG C of hydro-thermal reactions are moved into
White depositions are obtained after 60min, Jing absolute ethyl alcohols and deionized water alternating centrifugal are cleaned 3 times, filtered, and drying is spent
Shape ZnO nanorod.
2) by 0.15g KI and 0.56g Bi (NO3)3·5H2O is added in 30mL ethylene glycol, magnetic agitation 50min, then is added
Enter 0.3g by step 1) the flower-shaped ZnO nanorod that obtains, ultrasonic disperse 20min, in pouring autoclave into, 110 DEG C of solvent heats
Reaction 1h, Jing absolute ethyl alcohols and deionized water alternating centrifugal are cleaned 3 times, are filtered, and drying obtains flaxen flakes ZnO/
BiOI composites.
Photocatalytic degradation is tested：
Nanometer BiOI and nano-ZnO (Fig. 1) and each 10mg of ZnO/BiOI (Fig. 2) prepared by above-described embodiment are weighed,
And be added in rhodamine degradation solution (50mL, 5mg/L) respectively as photochemical catalyst, ultrasonic disperse 20min.Open magnetic agitation
Device, dark reaction 1h, in this, as initial time zero point, using ultraviolet-visible spectrophotometer rhodamine is tested up to absorption-balance
The absorbance of solution.Then, xenon source (500W) is opened, under continuing magnetic force stirring light-catalyzed reaction is carried out, every 1h samplings
And centrifuging and taking supernatant liquor, determine the absorbance of solution.
Referring to Fig. 3, illumination 2h under visible light is can be seen that from the photocatalysis effect of photocatalytic degradation rhodamine liquor
Afterwards, nano-ZnO, BiOI and ZnO/BiOI photochemical catalysts to the degradation rate of rhodamine liquor respectively up to 5%, 37% and 92%.With
Other patterns are compared, and flakes ZnO/BiOI composites are to form closelypacked stratiform BiOI on the surface of ZnO nanorod
Spheroid, photocatalytic activity is significantly improved.
In a word, ZnO nanorod and visible ray optical Response preferably BiOI are carried out compound preparation ZnO/BiOI by the present invention
Composite, at the same by Effective Regulation BiOI spheroids ZnO nanorod surface load capacity and distributing homogeneity, and then improve
The photocatalytic activity of composite affects, and solvent-thermal method easily controllable reaction time, reaction temperature, and equipment is simple, cost
It is low.Research of the present invention to the photocatalytic activity of ZnO/BiOI compounds has great importance.
Claims (8)
1. a kind of preparation method of flakes ZnO/BiOI composites, it is characterised in that：Comprise the following steps：
1) by Zn (NO3)3·6H2O and NaOH are dissolved in deionized water, obtain mixed liquor A, and lauryl sodium sulfate is scattered in into nothing
In the mixed solvent of water-ethanol and deionized water, mixed liquid B is obtained, 30～40min, Ran Houjin will be stirred after mixed liquor A and B mixing
Row microwave radiation technology hydro-thermal reaction, the sediment that reaction is obtained is scrubbed and dries, and obtains flower-shaped ZnO nanorod；
2) by KI and Bi (NO3)3·5H2O is stirred to being uniformly dispersed after adding in ethylene glycol, obtains mixed liquor C, is added in mixed liquor C
Enter ultrasonic disperse after the flower-shaped ZnO nanorod that step 1 is obtained, then carry out solvent thermal reaction, precipitate after reaction it is scrubbed and
Drying, obtains flakes ZnO/BiOI composites.
2. a kind of preparation method of flakes ZnO/BiOI composites as claimed in claim 1, it is characterised in that：It is described mixed
In closing liquid A, Zn (NO3)3·6H2The consumption of O is 0.1～0.9g, and the consumption of NaOH is 0.3～2.5g, and the consumption of deionized water is
1～5mL；In the mixed liquid B, the consumption of lauryl sodium sulfate is 0.1～3g, and the consumption of deionized water is 10～300mL,
The consumption of absolute ethyl alcohol is 1～50mL.
3. a kind of preparation method of flakes ZnO/BiOI composites as claimed in claim 1, it is characterised in that be：Institute
The reaction temperature for stating microwave radiation technology hydro-thermal reaction is 100～180 DEG C, and the reaction time is 30～60min.
4. a kind of preparation method of flakes ZnO/BiOI composites as claimed in claim 1, it is characterised in that be：Institute
In stating mixed liquor C, the consumption of KI is 0.08～0.2g, Bi (NO3)3·5H2The consumption of O be 0.3～0.6g, the consumption of ethylene glycol
For 10～40mL；The addition of flower-shaped ZnO nanorod is 0.05～0.3g in the mixed liquor C.
5. a kind of preparation method of flakes ZnO/BiOI composites as claimed in claim 1, it is characterised in that：The step
In rapid 2, mixing time is 35～60min.
6. a kind of preparation method of flakes ZnO/BiOI composites as claimed in claim 1, it is characterised in that：The step
In rapid 2, the ultrasonic disperse time is 15～30min.
7. a kind of preparation method of flakes ZnO/BiOI composites as claimed in claim 1, it is characterised in that be：Institute
The reaction temperature for stating solvent thermal reaction is 110～160 DEG C, and the reaction time is 1h～3h.
8. a kind of preparation method of flakes ZnO/BiOI composites as claimed in claim 1, it is characterised in that be：Institute
In stating step 1, the temperature of drying is 60～70 DEG C；In the step 2, the temperature of drying is 80～90 DEG C.
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| CN108311162A (en) * | 2018-02-06 | 2018-07-24 | 常州大学 | A kind of preparation method and applications of ZnO/BiOI heterojunction photocatalysts |
| CN108722392A (en) * | 2018-04-04 | 2018-11-02 | 菏泽学院 | A kind of preparation method of flakes Zn-Bi-Al ternary photocatalyst materials |
| CN109999859A (en) * | 2019-03-13 | 2019-07-12 | 东北大学 | A kind of preparation method of microspheroidal ZnO-BiOI composite material |
| CN110016681A (en) * | 2019-05-16 | 2019-07-16 | 西北师范大学 | A kind of ternary semiconductor lamination complex light electrode and its preparation method and application |
| CN110075877A (en) * | 2019-03-26 | 2019-08-02 | 东北大学 | A kind of preparation method of ZnO-BiOI composite photo-catalyst |
| CN111013562A (en) * | 2019-11-20 | 2020-04-17 | 西安建筑科技大学 | ZnO/in (OH) with different shapes3Preparation method of composite photocatalyst |
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| CN112844425A (en) * | 2021-01-30 | 2021-05-28 | 哈尔滨商业大学 | C/ZnO/BiOI ternary composite photocatalytic material |
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| CN108311162A (en) * | 2018-02-06 | 2018-07-24 | 常州大学 | A kind of preparation method and applications of ZnO/BiOI heterojunction photocatalysts |
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| CN108722392B (en) * | 2018-04-04 | 2019-03-19 | 菏泽学院 | A kind of preparation method of flakes Zn-Bi-Al ternary photocatalyst material |
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| CN111013562B (en) * | 2019-11-20 | 2023-03-31 | 西安建筑科技大学 | ZnO/In (OH) with different shapes 3 Preparation method of composite photocatalyst |
| CN112264079A (en) * | 2020-11-23 | 2021-01-26 | 景德镇陶瓷大学 | Method for constructing metal oxide nano array/two-dimensional carbon nitride |
| CN112844425A (en) * | 2021-01-30 | 2021-05-28 | 哈尔滨商业大学 | C/ZnO/BiOI ternary composite photocatalytic material |
| CN114029062A (en) * | 2021-11-23 | 2022-02-11 | 天津工业大学 | Preparation method of oxygen-enriched vacancy multivalent cobalt in-situ doped ZnO flower-like microsphere composite photocatalyst |
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