CN107235506B - A kind of preparation method of nano zine oxide heterojunction structure - Google Patents
A kind of preparation method of nano zine oxide heterojunction structure Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 45
- 238000006243 chemical reaction Methods 0.000 claims abstract description 22
- 239000011787 zinc oxide Substances 0.000 claims abstract description 22
- 239000002135 nanosheet Substances 0.000 claims abstract description 16
- MSNWSDPPULHLDL-UHFFFAOYSA-K ferric hydroxide Chemical compound [OH-].[OH-].[OH-].[Fe+3] MSNWSDPPULHLDL-UHFFFAOYSA-K 0.000 claims abstract description 15
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 13
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 45
- 239000000047 product Substances 0.000 claims description 38
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 33
- 235000019441 ethanol Nutrition 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 10
- 229910016874 Fe(NO3) Inorganic materials 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 7
- 230000032683 aging Effects 0.000 claims description 5
- 238000003760 magnetic stirring Methods 0.000 claims description 5
- 239000006227 byproduct Substances 0.000 claims description 4
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 3
- 239000011701 zinc Substances 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims 1
- 229910052760 oxygen Inorganic materials 0.000 claims 1
- 239000001301 oxygen Substances 0.000 claims 1
- 238000009423 ventilation Methods 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 7
- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 abstract description 4
- 238000001354 calcination Methods 0.000 abstract description 3
- 239000003463 adsorbent Substances 0.000 abstract description 2
- 239000003054 catalyst Substances 0.000 abstract description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 abstract description 2
- 239000002086 nanomaterial Substances 0.000 abstract description 2
- 239000002245 particle Substances 0.000 abstract description 2
- 238000012827 research and development Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 14
- 239000000243 solution Substances 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 9
- 230000015556 catabolic process Effects 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 5
- 238000000576 coating method Methods 0.000 description 5
- 238000006731 degradation reaction Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- MCPLVIGCWWTHFH-UHFFFAOYSA-L methyl blue Chemical compound [Na+].[Na+].C1=CC(S(=O)(=O)[O-])=CC=C1NC1=CC=C(C(=C2C=CC(C=C2)=[NH+]C=2C=CC(=CC=2)S([O-])(=O)=O)C=2C=CC(NC=3C=CC(=CC=3)S([O-])(=O)=O)=CC=2)C=C1 MCPLVIGCWWTHFH-UHFFFAOYSA-L 0.000 description 3
- 229960000907 methylthioninium chloride Drugs 0.000 description 3
- 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 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 2
- 235000013339 cereals Nutrition 0.000 description 2
- RLGQACBPNDBWTB-UHFFFAOYSA-N cetyltrimethylammonium ion Chemical compound CCCCCCCCCCCCCCCC[N+](C)(C)C RLGQACBPNDBWTB-UHFFFAOYSA-N 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- AGBXYHCHUYARJY-UHFFFAOYSA-N 2-phenylethenesulfonic acid Chemical compound OS(=O)(=O)C=CC1=CC=CC=C1 AGBXYHCHUYARJY-UHFFFAOYSA-N 0.000 description 1
- MKYBYDHXWVHEJW-UHFFFAOYSA-N N-[1-oxo-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propan-2-yl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(C(C)NC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 MKYBYDHXWVHEJW-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 description 1
- 229960000250 adipic acid Drugs 0.000 description 1
- 235000011037 adipic acid Nutrition 0.000 description 1
- 125000004397 aminosulfonyl group Chemical group NS(=O)(=O)* 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- KTUQUZJOVNIKNZ-UHFFFAOYSA-N butan-1-ol;hydrate Chemical compound O.CCCCO KTUQUZJOVNIKNZ-UHFFFAOYSA-N 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000011538 cleaning material Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 125000005395 methacrylic acid group Chemical group 0.000 description 1
- 239000004530 micro-emulsion Substances 0.000 description 1
- 239000011943 nanocatalyst Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000004246 zinc acetate Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/02—Oxides; Hydroxides
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/80—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with 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
- 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
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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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/40—Catalysts, in general, characterised by their form or physical properties characterised by dimensions, e.g. grain size
-
- 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
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/06—Ferric oxide [Fe2O3]
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2006/12—Surface area
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Abstract
The present invention relates to the research and development technology fields of nano material, disclose a kind of preparation method of nano zine oxide heterojunction structure, include the following steps：Step（1）And step（2）Zinc oxide nano sheet is prepared using simple hydro-thermal reaction, reduces reaction cost, in the form of sheets, size is inhomogenous for nano zine oxide structure at this time；Step（3）Ferric hydroxide gel is prepared using sol-gal process, there is high specific surface area, be the adsorbent of excellent catalyst carrier or function admirable；（3）The Zinc oxide nano sheet that will be obtained, is distributed in ferric hydroxide gel, and ZnO/a Fe2O3 nano-heterogeneous structures are prepared in calcining, and particle is in short cylinder or club shaped structure, and grain size is uniformly distributed in 80 ran ranges, has fabulous photocatalytic degradation.
Description
Technical field
The invention belongs to the research and development technology fields of nano material, and in particular to a kind of preparation of nano zine oxide heterojunction structure
Method.
Background technology
Nano zine oxide is as a kind of high-performance semiconductor material since it is with unique small-size effect, surface effect
It answers, quantum size effect, macro quanta tunnel effect and Dielectric confinement effect, therefore in anti-biotic material, luminescent material, piezoresistive material
There is very extensive application in material, ultraviolet shielding material, self-cleaning material, cell calibration material and nanocatalyst etc. fields
Foreground.Characteristic possessed by zinc oxide nano-particle has more close relationship with the physical features of its own.How to select to close
Suitable coating material prepares the controllable nano zinc oxide material of size and shape by solution chemical processes, expands its application
Field, the fabulous nanometer product of the performance that is applied are one of the hot issues of current nano zinc oxide material research.
Research at present for nano zine oxide in catalytic degradation technology field is also still immature, does not obtain substantially preferably
Application have very important significance for the recycling tool of environmental pollution resource there is huge development space.
Invention content
The purpose of the present invention is for existing problem, providing a kind of preparation method of nano zine oxide heterojunction structure,
Zinc oxide nano sheet is obtained using simple hydro-thermal reaction method, is distributed in ferric hydroxide gel, ZnO/a- is prepared in calcining
Fe2O3Nano-heterogeneous structure, grain size are uniformly distributed in 80 ran ranges, have fabulous photocatalytic degradation.
The present invention is achieved by the following technical solutions：
A kind of preparation method of nano zine oxide heterojunction structure, includes the following steps：
（1）It weighs 0.1-0.15 moles of zinc nitrate to be placed in 100 milliliters of beakers, molar concentration is added and rubs for 0.2-0.3
You/liter sodium hydroxide solution, addition is subject to solution ph and reaches 8.0-8.2, and 15-20 points are stirred under magnetic stirring apparatus
Clock, adds 10-15 ml deionized water ultrasonic disperses 20-30 minutes, obtains solid-liquid mixture；
（2）Solid-liquid mixture after ultrasonic disperse is persistently stirred 15-20 minutes, is then transferred in hydrothermal reaction kettle,
180-200 DEG C is reacted 18-20 hours, is taken out reaction kettle and is placed in cooled to room temperature in draught cupboard, removes product, product is used
Ethyl alcohol and deionized water are washed 3-5 times respectively, obtain product, then product is placed in drying 8-10 hours in 60-70 DEG C of baking oven, so
After be put into Muffle furnace and calcine 1-2 hours to get Zinc oxide nano sheet；
（3）0.2-0.3 moles of Fe(NO3)39H2O is weighed, 10-15 milliliters of ethyl alcohol dissolving is added, according to nine hydration nitre
Sour iron is 1 with sodium hydroxide molar ratio：（3-3.5）Ratio sodium hydroxide is added, mixed liquor is put into after being sufficiently stirred closed
In insulating box, isothermal reaction 2-3 hours at 45-55 DEG C, aging 10-12 hours at room temperature, ferric hydroxide gel is obtained；
（4）The Zinc oxide nano sheet being prepared is added in ferric hydroxide gel, under 300-350 revs/min, is held
Continuous stirring 40-50 minutes, is then transferred in hydrothermal reaction kettle, and 160-180 DEG C is reacted 20-22 hours, takes out reaction kettle and is placed in
Cooled to room temperature in draught cupboard removes product and washs product ethyl alcohol and deionized water 3-5 times respectively, obtains product,
Product is placed in drying 12-15 hours in 60-70 DEG C of baking oven again, is then placed in calcine 2-3 hours in Muffle furnace and be received to get described
The zinc oxide heterogeneous structure of rice.
As further improvement of these options, the ethanol solution used in preparation is that analysis is pure.
The present invention has the following advantages compared with prior art：In order to solve nano zine oxide present in preparation in solvent
Post-processing, coating material molecular structure is complicated, of high cost, reaction condition is complicated, and the high and property that consumes energy in reaction process is not convex
Aobvious unstable problem, the present invention provides a kind of preparation methods of nano zine oxide heterojunction structure, include the following steps：Step
（1）And step（2）Zinc oxide nano sheet is prepared using simple hydro-thermal reaction, reduces reaction cost, at this time nano oxidized
In the form of sheets, size is inhomogenous for zinc structure；Step（3）Ferric hydroxide gel is prepared using sol-gel method, there is pole
High specific surface area is the adsorbent of excellent catalyst carrier or function admirable, after being combined with Zinc oxide nano sheet, profit
With it there is very high adsorption capacity and visible light to drive the characteristic of photocatalytic degradation cation organic pollution, environmental pollution
Improvement have prodigious application value；（3）The Zinc oxide nano sheet that will be obtained, is distributed in ferric hydroxide gel, prepared by calcining
Obtain ZnO/a-Fe2O3Nano-heterogeneous structure, particle are in short cylinder or club shaped structure, and grain size uniformly divides in 80 ran ranges
Cloth has fabulous photocatalytic degradation.
Specific implementation mode
With reference to specific embodiment, the present invention will be further described.
Embodiment 1
A kind of preparation method of nano zine oxide heterojunction structure, includes the following steps：
（1）It weighs 0.1 mole of zinc nitrate to be placed in 100 milliliters of beakers, the hydrogen that molar concentration is 0.2 mol/L is added
Sodium hydroxide solution, addition are subject to solution ph and reach 8.0, stirred 15 minutes under magnetic stirring apparatus, add 10 milliliters
Deionized water ultrasonic disperse 20 minutes, obtains solid-liquid mixture；
（2）Solid-liquid mixture after ultrasonic disperse is persistently stirred 15 minutes, is then transferred in hydrothermal reaction kettle, 180
DEG C reaction 18 hours, takes out reaction kettle and is placed in cooled to room temperature in draught cupboard, remove product, by product ethyl alcohol and go from
Sub- water washs 3 times respectively, obtains product, then product is placed in drying 8 hours in 60 DEG C of baking ovens, is then placed in Muffle furnace and calcines
1 hour to get Zinc oxide nano sheet；
（3）Weigh 0.2 mole of Fe(NO3)39H2O, 10 milliliters of ethyl alcohol dissolving be added, according to Fe(NO3)39H2O with
Sodium hydroxide molar ratio is 1：Sodium hydroxide is added in 3 ratio, mixed liquor is put into closed insulating box after being sufficiently stirred, 45
Isothermal reaction 2 hours at DEG C, aging 10 hours, obtain ferric hydroxide gel at room temperature；
（4）The Zinc oxide nano sheet being prepared is added in ferric hydroxide gel, under 300 revs/min, is persistently stirred
It mixes 400 minutes, is then transferred in hydrothermal reaction kettle, 160 DEG C are reacted 20 hours, and taking-up reaction kettle is placed in naturally cold in draught cupboard
But it to room temperature, removes product and washs product ethyl alcohol and deionized water respectively 3 times, obtain product, then product is placed in 60 DEG C
It is 12 hours dry in baking oven, it is then placed in Muffle furnace and calcines 2 hours to get the nano zine oxide heterojunction structure.
Embodiment 2
A kind of preparation method of nano zine oxide heterojunction structure, includes the following steps：
（1）It weighs 0.12 mole of zinc nitrate to be placed in 100 milliliters of beakers, it is 0.25 mol/L that molar concentration, which is added,
Sodium hydroxide solution, addition are subject to solution ph and reach 8.1, stirred 18 minutes under magnetic stirring apparatus, add 13 millis
It rises deionized water ultrasonic disperse 25 minutes, obtains solid-liquid mixture；
（2）Solid-liquid mixture after ultrasonic disperse is persistently stirred 17 minutes, is then transferred in hydrothermal reaction kettle, 190
DEG C reaction 19 hours, takes out reaction kettle and is placed in cooled to room temperature in draught cupboard, remove product, by product ethyl alcohol and go from
Sub- water washs 4 times respectively, obtains product, then product is placed in drying 9 hours in 65 DEG C of baking ovens, is then placed in Muffle furnace and calcines
1.5 hours to get Zinc oxide nano sheet；
（3）Weigh 0.25 mole of Fe(NO3)39H2O, 12 milliliters of ethyl alcohol dissolving be added, according to Fe(NO3)39H2O with
Sodium hydroxide molar ratio is 1：Sodium hydroxide is added in 3.2 ratio, and mixed liquor is put into closed insulating box after being sufficiently stirred,
Isothermal reaction 2.5 hours at 50 DEG C, aging 11 hours, obtain ferric hydroxide gel at room temperature；
（4）The Zinc oxide nano sheet being prepared is added in ferric hydroxide gel, under 320 revs/min, is persistently stirred
It mixes 45 minutes, is then transferred in hydrothermal reaction kettle, 170 DEG C are reacted 21 hours, and taking-up reaction kettle is placed in naturally cold in draught cupboard
But it to room temperature, removes product and washs product ethyl alcohol and deionized water respectively 4 times, obtain product, then product is placed in 65 DEG C
It is 13 hours dry in baking oven, it is then placed in Muffle furnace and calcines 2.5 hours to get the nano zine oxide heterojunction structure.
Embodiment 3
A kind of preparation method of nano zine oxide heterojunction structure, includes the following steps：
（1）It weighs 0.15 mole of zinc nitrate to be placed in 100 milliliters of beakers, the hydrogen that molar concentration is 0.3 mol/L is added
Sodium hydroxide solution, addition are subject to solution ph and reach 8.2, stirred 20 minutes under magnetic stirring apparatus, add 15 milliliters
Deionized water ultrasonic disperse 30 minutes, obtains solid-liquid mixture；
（2）Solid-liquid mixture after ultrasonic disperse is persistently stirred 20 minutes, is then transferred in hydrothermal reaction kettle, 200
DEG C reaction 20 hours, takes out reaction kettle and is placed in cooled to room temperature in draught cupboard, remove product, by product ethyl alcohol and go from
Sub- water washs 5 times respectively, obtains product, then product is placed in drying 10 hours in 70 DEG C of baking ovens, is then placed in Muffle furnace and forges
2 hours are burnt to get Zinc oxide nano sheet；
（3）Weigh 0.3 mole of Fe(NO3)39H2O, 15 milliliters of ethyl alcohol dissolving be added, according to Fe(NO3)39H2O with
Sodium hydroxide molar ratio is 1：Sodium hydroxide is added in 3.5 ratio, and mixed liquor is put into closed insulating box after being sufficiently stirred,
Isothermal reaction 3 hours at 55 DEG C, aging 12 hours, obtain ferric hydroxide gel at room temperature；
（4）The Zinc oxide nano sheet being prepared is added in ferric hydroxide gel, under 350 revs/min, is persistently stirred
It mixes 50 minutes, is then transferred in hydrothermal reaction kettle, 180 DEG C are reacted 22 hours, and taking-up reaction kettle is placed in naturally cold in draught cupboard
But it to room temperature, removes product and washs product ethyl alcohol and deionized water respectively 5 times, obtain product, then product is placed in 70 DEG C
It is 15 hours dry in baking oven, it is then placed in Muffle furnace and calcines 3 hours to get the nano zine oxide heterojunction structure.
Comparative example 1
Nano zine oxide is prepared using solution chemical method, using aminosulfonyl base class, methacrylic, styrene sulfonic acid
The existing organic polymer such as class is as coating material.
Comparative example 2
Using zinc acetate, hexanedioic acid as primary raw material, cetyl trimethyl ammonium is coating material, solidifying using colloidal sol-
Glue method prepares nano zine oxide.
Comparative example 3
Using normal octane as primary raw material, using cetyl trimethyl ammonium as coating material, n-butanol is that surface is helped to repair
Agent is adornd, nano zine oxide is prepared in n-butanol-water microemulsion system.
Comparative example 4
With differing only in for embodiment 2, by step（3）And step（4）Process omit, remaining is consistent.
Contrast test
The method of embodiment 1-3 and comparative example 1-4 is used to prepare nano oxidized zinc product respectively, every group takes 3 parts of samples,
Every group of sample is placed in aqueous solution of methylene blue, methyl blue aqueous solution, rhodamine aqueous solution respectively, it is anti-under ultraviolet light
It answers 2 hours, measures the degradation rate of methylene blue, methyl blue and rhodamine, logging is as shown in the table：
| Project | Methylene blue degradation rate（%） | Methyl blue degradation rate（%） | Rhodamine degradation rate（%） | Specific surface area（m2/g） |
| Embodiment 1 | 92.5 | 93.6 | 96.4 | 88 |
| Embodiment 2 | 93.4 | 94.7 | 97.5 | 89 |
| Embodiment 3 | 92.8 | 94.2 | 96.8 | 88 |
| Comparative example 1 | 84.2 | 85.4 | 87.1 | 82 |
| Comparative example 2 | 82.6 | 84.3 | 85.9 | 80 |
| Comparative example 3 | 80.5 | 82.5 | 84.3 | 79 |
| Comparative example 4 | 75.8 | 78.4 | 80.2 | 75 |
As seen from the experiment：Nano zine oxide heterojunction structure prepared by the present invention has fabulous photocatalytic degradation,
There is prodigious application prospect in environmental contaminants improvement.
Claims (1)
1. a kind of preparation method of nano zine oxide heterojunction structure, which is characterized in that include the following steps：
（1）It weighs 0.1-0.15 moles of zinc nitrate to be placed in 100 milliliters of beakers, addition molar concentration is 0.2-0.3 mol/Ls
Sodium hydroxide solution, addition is subject to solution ph and reaches 8.0-8.2, stirred 15-20 minutes under magnetic stirring apparatus, then
10-15 ml deionized water ultrasonic disperses are added 20-30 minutes, obtain solid-liquid mixture；
（2）Solid-liquid mixture after ultrasonic disperse is persistently stirred 15-20 minutes, is then transferred in hydrothermal reaction kettle, 180-
200 DEG C are reacted 18-20 hours, are taken out reaction kettle and are placed in cooled to room temperature in draught cupboard, product are removed, by product ethyl alcohol
It is washed 3-5 times respectively with deionized water, obtains product, then product is placed in drying 8-10 hours in 60-70 DEG C of baking oven, then put
Enter to calcine 1-2 hours in Muffle furnace to get Zinc oxide nano sheet；
（3）0.2-0.3 moles of Fe(NO3)39H2O is weighed, 10-15 milliliters of ethyl alcohol dissolving is added, according to Fe(NO3)39H2O
It is 1 with sodium hydroxide molar ratio：（3-3.5）Ratio be added sodium hydroxide, mixed liquor is put into closed constant temperature after being sufficiently stirred
In case, isothermal reaction 2-3 hours at 45-55 DEG C, aging 10-12 hours at room temperature, ferric hydroxide gel is obtained；
（4）The Zinc oxide nano sheet being prepared is added in ferric hydroxide gel, under 300-350 revs/min, is persistently stirred
It mixes 40-50 minutes, is then transferred in hydrothermal reaction kettle, 160-180 DEG C is reacted 20-22 hours, is taken out reaction kettle and is placed in ventilation
Cooled to room temperature in cupboard removes product and washs product ethyl alcohol and deionized water 3-5 times respectively, obtains product, then will
Product is placed in drying 12-15 hours in 60-70 DEG C of baking oven, is then placed in Muffle furnace and calcines 2-3 hours to get the nano oxygen
Change zinc heterojunction structure.
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| CN111422899B (en) * | 2020-05-26 | 2022-12-02 | 安徽锦华氧化锌有限公司 | Preparation method of nano zinc oxide-vanadium oxide composite material |
| CN111584849B (en) * | 2020-05-26 | 2022-03-22 | 安徽锦华氧化锌有限公司 | Nano zinc oxide composite material applied to secondary battery |
| CN114518390B (en) * | 2020-11-20 | 2023-06-06 | 中国科学院大连化学物理研究所 | Porous zinc oxide sensor, preparation method and application |
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