CN106563411B - A kind of preparation method of flakes ZnO/BiOI composite material - Google Patents
A kind of preparation method of flakes ZnO/BiOI composite material Download PDFInfo
- Publication number
- CN106563411B CN106563411B CN201610986384.8A CN201610986384A CN106563411B CN 106563411 B CN106563411 B CN 106563411B CN 201610986384 A CN201610986384 A CN 201610986384A CN 106563411 B CN106563411 B CN 106563411B
- Authority
- CN
- China
- Prior art keywords
- zno
- flakes
- composite material
- bioi
- dosage
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 239000002131 composite material Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 32
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 30
- 239000008367 deionised water Substances 0.000 claims abstract description 30
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 30
- 239000002073 nanorod Substances 0.000 claims abstract description 26
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
- 229960000935 dehydrated alcohol Drugs 0.000 claims abstract description 19
- 239000002904 solvent Substances 0.000 claims abstract description 12
- 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
- 239000000203 mixture Substances 0.000 claims abstract 2
- 238000001035 drying Methods 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 239000012046 mixed solvent Substances 0.000 claims description 2
- 238000002156 mixing Methods 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
- 238000013019 agitation Methods 0.000 abstract description 13
- 239000000243 solution Substances 0.000 abstract description 10
- 230000001699 photocatalysis Effects 0.000 abstract description 9
- 238000000034 method Methods 0.000 abstract description 8
- 239000011259 mixed solution Substances 0.000 abstract description 7
- 150000001875 compounds Chemical class 0.000 description 10
- 238000001914 filtration Methods 0.000 description 10
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 8
- 238000000151 deposition Methods 0.000 description 5
- 230000008021 deposition Effects 0.000 description 5
- 238000007146 photocatalysis Methods 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
- 239000000463 material Substances 0.000 description 3
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 3
- RZYKUPXRYIOEME-UHFFFAOYSA-N CCCCCCCCCCCC[S] Chemical compound CCCCCCCCCCCC[S] RZYKUPXRYIOEME-UHFFFAOYSA-N 0.000 description 2
- 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 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
- 238000005286 illumination Methods 0.000 description 2
- 239000002121 nanofiber Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 239000000126 substance 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
- 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
- 230000007613 environmental effect Effects 0.000 description 1
- 229960004756 ethanol Drugs 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 238000002474 experimental method Methods 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
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 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
- 238000011160 research Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000012360 testing method Methods 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
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
- 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
-
- 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
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- 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
-
- 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
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Hydrology & Water Resources (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a kind of preparation methods of flakes ZnO/BiOI composite material, first by Zn (NO3)3·6H2O and NaOH are dissolved in deionized water, then disperse lauryl sodium sulfate in dehydrated alcohol and the mixed solution of deionized water, then mix both the above solution, after magnetic agitation, obtain flower-shaped ZnO nanorod using microwave-assisted hydro-thermal method.By KI and Bi (NO3)3·5H2O is added in ethylene glycol, and magnetic agitation for a period of time, adds the flower-shaped ZnO nanorod prepared, ultrasonic disperse, obtains flaxen flakes ZnO/BiOI composite material after solvent thermal reaction.Compared with other patterns, flakes ZnO/BiOI composite material is to form closelypacked stratiform BiOI sphere on the surface of ZnO nanorod, and photocatalytic activity significantly improves.And solvent-thermal method easily controllable reaction time, reaction temperature, equipment is simple, at low cost.
Description
Technical field
The present invention relates to a kind of preparation methods of flakes ZnO/BiOI composite material.
Background technique
The bismuth oxyhalide (BiOX, X-F, Cl, Br, I) of layer structure is used as a new class of semiconductor light-catalyst, with
Its good Uv and visible light optical Response and be concerned.For BiOI as one of bismuth oxyhalide, band gap is narrow
(1.77-1.92eV) shows preferable absorption characteristic in visible-range, has excellent photocatalysis under visible light illumination
Degradation property, but the photo-generate electron-hole of pure BiOI is easily compound, and semiconductors coupling rule can effectively inhibit light
The recombination rate of raw carrier, so that the separation rate of carrier is improved, conducive to the photocatalysis performance for improving substance.
Wang etc. (Wang S, Guan Y, Wang L.Applied Catalysis B:Environmental, 2015,
168:448-457.) using ethylene glycol as solvent, BiOI/Ag is prepared for by chemical precipitation process using solvent-thermal method3VO4It is compound
Material, in contrast, the visible light photocatalysis active of the compound are much better than single Ag, Ag3VO4And BiOI.Liao etc.
(Liao C, Ma Z, Dong G.Applied Surface Science, 2014,314:481-489.) is repaired with BiOI nanometer sheet
Adorn TiO2Nanofiber prepares composite material, is cut by controlling the source Bi concentration between the modification two kinds of substances, BiOI exists
TiO2Nanofiber surface is uniformly distributed, and has very high visible light catalysis activity.(Dai K, the Lu L, Liang such as Dai
C.Dalton Transactions, 2015,44:7903-7910.) in ethyl alcohol and the mixed solution of deionized water, using water
Thermal method is prepared for coaxial C3N4/ BiOI/graphene oxide heterogeneous material compound, the compound of three effectively inhibit photoproduction
Electron-hole it is compound, to improve the catalytic performance of material.
Currently, there is not yet the report of the preparation method about flakes ZnO/BiOI composite material.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of flakes ZnO/BiOI composite material.
To achieve the goals above, the invention adopts the following technical scheme:
1) by Zn (NO3)3·6H2O and NaOH are dissolved in deionized water, obtain mixed liquor A, and lauryl sodium sulfate is dispersed
In the in the mixed solvent of dehydrated alcohol and deionized water, mixed liquid B is obtained, stirs 30~40min after mixed liquor A and B are mixed, so
Microwave assisted aqueous extraction thermal response is carried out afterwards, and the sediment that reaction is obtained is washed and dries, and obtains flower-shaped ZnO nanorod；
2) by KI and Bi (NO3)3·5H2Stirring obtains mixed liquor C, to mixed liquor C to being uniformly dispersed after O is added in ethylene glycol
Middle ultrasonic disperse after the obtained flower-shaped ZnO nanorod of step 1 is added, then carries out solvent thermal reaction, after reaction through washing and
Drying, obtains flakes ZnO/BiOI composite material.
In the mixed liquor A, Zn (NO3)3·6H2The dosage of O is 0.1~0.9g, and the dosage of NaOH is 0.3~2.5g, is gone
The dosage of ionized water is 1~5mL；In the mixed liquid B, the dosage of lauryl sodium sulfate is 0.1~3g, the use of deionized water
Amount is 10~300mL, and the dosage of dehydrated alcohol is 1~50mL.
The reaction temperature of the microwave-assisted hydro-thermal reaction is 100~180 DEG C, and the reaction time is 30~60min.
In the mixed liquor C, the dosage of KI is 0.08~0.2g, Bi (NO3)3·5H2The dosage of O is 0.3~0.6g, second
The dosage of glycol is 10~40mL；The additional amount 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 invention has the following beneficial effects:
The present invention is on the basis of being prepared ZnO nanorod, with Bi (NO3)3·5H2O and KI is raw material, in ethylene glycol
In solvent, flakes ZnO/BiOI composite material is prepared for using solvent-thermal method, simple process, reaction temperature and reaction time is easy
Control, it is low in cost.Flakes ZnO/BiOI compound is to prepare spherical BiOI on ZnO nanorod surface, and the composite material is big
Specific surface area, adsorptivity both can be improved, its visible light photocatalysis active can also be promoted, and be used to prepare high catalytic activity
BiOI also there is very big prospect.
Detailed description of the invention
Fig. 1 is the SEM stereoscan photograph of flower-shaped ZnO nanorod；In Fig. 1, scale is 4 μm.
Fig. 2 is the stereoscan photograph of flakes ZnO/BiOI compound；In Fig. 2, scale is 2 μm.
Fig. 3 is the photocatalytic degradation capability curve of ZnO, BiOI and ZnO/BiOI (preparation of 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 to solution of the invention
It releases, rather than limits.
Embodiment 1:
1) by 0.5g Zn (NO3)3·6H2O and 1.5g NaOH is dissolved in 3mL deionized water, then by 1g dodecyl sulphate
Sodium (SDS) is scattered in the mixed solution of 100mL deionized water and 25mL dehydrated alcohol, then mixes both the above solution,
After magnetic agitation 30min, polytetrafluoroethyltank tank is moved into, is placed in the microwave dissolver of MDS-10 model, 180 DEG C of hydro-thermal reactions
White depositions are obtained after 40min, are cleaned 3 times through dehydrated alcohol and deionized water alternating centrifugal, and filtering is dried to get flower is arrived
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
The flower-shaped ZnO nanorod that 0.2g is obtained by step 1), ultrasonic disperse 20min are poured into autoclave, and 160 DEG C of solvent heats are anti-
3h is answered, is cleaned 3 times through dehydrated alcohol and deionized water alternating centrifugal, filtering is dried to get flaxen flakes ZnO/ is arrived
BiOI composite material.
Embodiment 2:
1) by 0.7g Zn (NO3)3·6H2O and 2.5g NaOH is dissolved in 4mL deionized water, then by 1.7g dodecyl sulphur
Sour sodium (SDS) is scattered in the mixed solution of 100mL deionized water and 30mL dehydrated alcohol, then mixes both the above solution
It closes, after magnetic agitation 30min, moves into polytetrafluoroethyltank tank, be placed in the microwave dissolver of MDS-10 model, 170 DEG C of hydro-thermals
Obtain white depositions after reaction 35min, cleaned 3 times through dehydrated alcohol and deionized water alternating centrifugal, filtering, drying to get
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
The flower-shaped ZnO nanorod that 0.2g is obtained by step 1), ultrasonic disperse 15min are poured into autoclave, and 130 DEG C of solvent heats are anti-
2h is answered, is cleaned 3 times through dehydrated alcohol and deionized water alternating centrifugal, filtering is dried to get flaxen flakes ZnO/ is arrived
BiOI composite material.
Embodiment 3:
1) by 0.3g Zn (NO3)3·6H2O and 1.0g NaOH is dissolved in 5mL deionized water, then by 2g dodecyl sulphate
Sodium (SDS) is scattered in the mixed solution of 150mL deionized water and 30mL dehydrated alcohol, then mixes both the above solution,
After magnetic agitation 30min, polytetrafluoroethyltank tank is moved into, is placed in the microwave dissolver of MDS-10 model, 150 DEG C of hydro-thermal reactions
White depositions are obtained after 35min, are cleaned 3 times through dehydrated alcohol and deionized water alternating centrifugal, and filtering is dried to get flower is arrived
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
The flower-shaped ZnO nanorod that 0.25g is obtained by step 1), ultrasonic disperse 25min are poured into autoclave, and 150 DEG C of solvent heats are anti-
3h is answered, is cleaned 3 times through dehydrated alcohol and deionized water alternating centrifugal, filtering is dried to get flaxen flakes ZnO/ is arrived
BiOI composite material.
Embodiment 4:
1) by 0.2g Zn (NO3)3·6H2O and 0.8g NaOH is dissolved in 3mL deionized water, then by 0.9g dodecyl sulphur
Sour sodium (SDS) is scattered in the mixed solution of 280mL deionized water and 30mL dehydrated alcohol, then mixes both the above solution
It closes, after magnetic agitation 30min, moves into polytetrafluoroethyltank tank, be placed in the microwave dissolver of MDS-10 model, 150 DEG C of hydro-thermals
Obtain white depositions after reaction 35min, cleaned 3 times through dehydrated alcohol and deionized water alternating centrifugal, filtering, drying to get
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 plus
Enter the flower-shaped ZnO nanorod that 0.28g is obtained by step 1), ultrasonic disperse 30min is poured into autoclave, 120 DEG C of solvent heats
2h is reacted, is cleaned 3 times through dehydrated alcohol and deionized water alternating centrifugal, filtering is dried to get flaxen flakes ZnO/ is arrived
BiOI composite material.
Embodiment 5:
1) by 0.6g Zn (NO3)3·6H2O and 1.2g NaOH is dissolved in 2mL deionized water, then by 2g dodecyl sulphate
Sodium (SDS) is scattered in the mixed solution of 180mL deionized water and 40mL dehydrated alcohol, then mixes both the above solution,
After magnetic agitation 30min, polytetrafluoroethyltank tank is moved into, is placed in the microwave dissolver of MDS-10 model, 160 DEG C of hydro-thermal reactions
White depositions are obtained after 60min, are cleaned 3 times through dehydrated alcohol and deionized water alternating centrifugal, and filtering is dried to get flower is arrived
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 plus
Enter the flower-shaped ZnO nanorod that 0.3g is obtained by step 1), ultrasonic disperse 20min is poured into autoclave, 110 DEG C of solvent heats
1h is reacted, is cleaned 3 times through dehydrated alcohol and deionized water alternating centrifugal, filtering is dried to get flaxen flakes ZnO/ is arrived
BiOI composite material.
Photocatalytic degradation experiment:
Nano-ZnO prepared by nanometer BiOI and above-described embodiment (Fig. 1) and ZnO/BiOI (Fig. 2) each 10mg are weighed,
And it is added in rhodamine degradation solution (50mL, 5mg/L) respectively as photochemical catalyst, ultrasonic disperse 20min.Open magnetic agitation
Device, dark reaction 1h reach absorption-balance, in this, as initial time zero point, test rhodamine using ultraviolet-visible spectrophotometer
The absorbance of solution.Then, xenon source (500W) is opened, continuing magnetic force stirring is lower to carry out light-catalyzed reaction, samples every 1h
And centrifuging and taking supernatant liquor, measure the absorbance of solution.
Referring to Fig. 3, illumination 2h under visible light can be seen that from the photocatalysis effect of photocatalytic degradation rhodamine liquor
Afterwards, nano-ZnO, BiOI and ZnO/BiOI photochemical catalyst are to the degradation rate of rhodamine liquor respectively up to 5%, 37% and 92%.With
Other patterns are compared, and flakes ZnO/BiOI composite material is to form closelypacked stratiform BiOI on the surface of ZnO nanorod
Sphere, photocatalytic activity significantly improve.
In short, ZnO nanorod and the preferable BiOI of visible light optical Response are carried out compound preparation ZnO/BiOI by the present invention
Composite material, while load capacity and distributing homogeneity by Effective Regulation BiOI sphere on ZnO nanorod surface, and then improve
The photocatalytic activity of composite material influences, and solvent-thermal method easily controllable reaction time, reaction temperature, and equipment is simple, cost
It is low.The present invention has great importance to the research of the photocatalytic activity of ZnO/BiOI compound.
Claims (7)
1. a kind of preparation method of flakes ZnO/BiOI composite material, it is characterised in that: the following steps are included:
1) by Zn (NO3)3·6H2O and NaOH are dissolved in deionized water, obtain mixed liquor A, disperse nothing for lauryl sodium sulfate
The in the mixed solvent of water-ethanol and deionized water, obtains mixed liquid B, will mixed liquor A and B mix after stir 30~40min, then into
The microwave-assisted hydro-thermal reaction of row, the sediment that reaction is obtained is washed and dries, and obtains flower-shaped ZnO nanorod；
2) by KI and Bi (NO3)3·5H2Stirring obtains mixed liquor C to being uniformly dispersed after O is added in ethylene glycol, adds into mixed liquor C
Enter ultrasonic disperse after the flower-shaped ZnO nanorod that step 1 obtains, then carries out solvent thermal reaction, the reaction of the solvent thermal reaction
Temperature is 130~160 DEG C, and the reaction time is 1h~3h, and washed and drying is precipitated after reaction, obtains flakes ZnO/BiOI
Composite material, flakes ZnO/BiOI composite material are to form closelypacked stratiform BiOI sphere on the surface of ZnO nanorod.
2. a kind of preparation method of flakes ZnO/BiOI composite material as described in claim 1, it is characterised in that: described mixed
It closes in liquid A, Zn (NO3)3·6H2The dosage of O is 0.1~0.9g, and the dosage of NaOH is 0.3~2.5g, and the dosage of deionized water is
1~5mL；In the mixed liquid B, the dosage of lauryl sodium sulfate is 0.1~3g, and the dosage of deionized water is 10~300mL,
The dosage of dehydrated alcohol is 1~50mL.
3. a kind of preparation method of flakes ZnO/BiOI composite material as described in claim 1, it is characterised in that be: institute
The reaction temperature for stating microwave-assisted 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 composite material as described in claim 1, it is characterised in that be: institute
It states in mixed liquor C, the dosage of KI is 0.08~0.2g, Bi (NO3)3·5H2The dosage of O is 0.3~0.6g, the dosage of ethylene glycol
For 10~40mL；The additional amount 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 composite material as described 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 composite material as described 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 composite material as described in claim 1, it is characterised in that be: institute
It states in step 1, the temperature of drying is 60~70 DEG C；In the step 2, the temperature of drying is 80~90 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610986384.8A CN106563411B (en) | 2016-11-09 | 2016-11-09 | A kind of preparation method of flakes ZnO/BiOI composite material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610986384.8A CN106563411B (en) | 2016-11-09 | 2016-11-09 | A kind of preparation method of flakes ZnO/BiOI composite material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106563411A CN106563411A (en) | 2017-04-19 |
| CN106563411B true CN106563411B (en) | 2019-05-10 |
Family
ID=58540882
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610986384.8A Active CN106563411B (en) | 2016-11-09 | 2016-11-09 | A kind of preparation method of flakes ZnO/BiOI composite material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106563411B (en) |
Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108311162A (en) * | 2018-02-06 | 2018-07-24 | 常州大学 | A kind of preparation method and applications of ZnO/BiOI heterojunction photocatalysts |
| 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 |
| CN109999859B (en) * | 2019-03-13 | 2020-04-03 | 东北大学 | Preparation method of microspherical ZnO-BiOI composite material |
| CN110075877A (en) * | 2019-03-26 | 2019-08-02 | 东北大学 | A kind of preparation method of ZnO-BiOI composite photo-catalyst |
| CN110016681B (en) * | 2019-05-16 | 2020-10-16 | 西北师范大学 | Ternary semiconductor laminated composite photoelectrode and preparation method and application thereof |
| 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 |
| CN114029062B (en) * | 2021-11-23 | 2024-02-02 | 天津工业大学 | Preparation method of oxygen-enriched vacancy multi-valence cobalt in-situ doped ZnO flower-like microsphere composite photocatalyst |
| CN115814817B (en) * | 2022-12-19 | 2024-06-07 | 长安大学 | Preparation method and application of ZnO@CuS piezoelectric-photocatalytic nanocomposite |
-
2016
- 2016-11-09 CN CN201610986384.8A patent/CN106563411B/en active Active
Non-Patent Citations (2)
| Title |
|---|
| Enhanced Photoelectrocatalytic Activity of BiOI Nanoplate-Zinc Oxide Nanorod p-n Heterojunction;Pan-Yong Kuang等;《Chem. Eur. J.》;20150901;第21卷;第15360–15368页 |
| Morphology-photocatalytic properties-growth mechanism for ZnO nanostructures via microwave-assisted hydrothermal synthesis;Jianzhong Ma等;《Cryst. Res. Technol.》;20130326;第48卷(第4期);第251–260页 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106563411A (en) | 2017-04-19 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106563411B (en) | A kind of preparation method of flakes ZnO/BiOI composite material | |
| CN104001496B (en) | A kind of BiVO 4nanometer sheet composite photocatalyst and its preparation method and application | |
| CN105148950A (en) | Preparing method for flower-shaped BiOI microspheres | |
| CN105664979A (en) | Nano-mesoporous micro-spherical Ln-Bi5O7I photocatalyst and preparation method thereof | |
| CN107376900A (en) | The preparation method and applications of bismuth molybdate ultrathin nanometer piece catalysis material | |
| CN107413354A (en) | A kind of preparation method for the cupric oxide nano composite for loading silver | |
| CN105056963B (en) | A kind of preparation method of di-iron trioxide doped cerium oxide nanometer rod composite material | |
| CN108993550A (en) | A kind of bromine oxygen bismuth photochemical catalyst and preparation method thereof that surface Lacking oxygen is modified | |
| CN103691433A (en) | Ag-doped TiO2 material, and preparation method and application thereof | |
| CN105540640A (en) | Preparation method of flower-shaped nanometer zinc oxide | |
| CN108355669A (en) | A kind of magnetic Nano onion carbon load Bi2WO6Photochemical catalyst and its preparation method and application | |
| CN104258857A (en) | Silver chromate-graphene oxide composite photocatalytic material and preparation method thereof | |
| CN105833917A (en) | Preparation method of silver-loaded titania nanotube-magnetic chitosan/beta-cyclodextrin composite material and application thereof | |
| CN105457656B (en) | The preparation method and purposes of a kind of heterojunction photocatalyst | |
| CN106902890A (en) | A kind of Cu BTC/ pucherites/SWCNTs ternary heterojunction structure photochemical catalysts and preparation method and application | |
| CN109529872A (en) | Amorphous nano titanium dioxide visible light catalyzer compound and preparation method thereof | |
| CN107159192A (en) | A kind of noble metal/TiO2Multilevel hierarchy of mixed crystal nanometer rods assembling and preparation method thereof | |
| CN104492464B (en) | Preparation method of silver iodide/beta type bismuth oxide composite material | |
| CN103990478A (en) | Preparation method of supported silver phosphate photocatalyst | |
| CN103894216A (en) | Preparation method of magnetic nano silver phosphate/titanium dioxide composite photocatalytic material | |
| CN102580720B (en) | Visible light response nano zinc oxide-bismuth oxide composite photocatalyst and preparation method thereof | |
| CN106955699B (en) | A kind of high-efficiency solar fixed nitrogen catalysis material and preparation method thereof | |
| Feng et al. | Novel visible-light-responding InVO4-Cu2O-TiO2 ternary nanoheterostructure: Preparation and photocatalytic characteristics | |
| CN105921153B (en) | A kind of composite photo-catalyst and preparation method thereof | |
| CN109395724A (en) | A kind of disilicic acid silver-TiO 2 visible light catalyst and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20230621 Address after: No. 355, Floor 4, Building 1, Phase I, Silk Road International Creative Dream Workshop, No. 3639, Ouya Avenue, Chanba Ecotope, Xi'an, Shaanxi 710021 [Cluster] Patentee after: Xi'an Huanchuang High-tech Development Co.,Ltd. Address before: No. 1, Weiyang District university garden, Xi'an, Shaanxi Province, Shaanxi Patentee before: SHAANXI University OF SCIENCE & TECHNOLOGY |
|
| TR01 | Transfer of patent right |