CN105540640B - Preparation method of flower-shaped nanometer zinc oxide - Google Patents
Preparation method of flower-shaped nanometer zinc oxide Download PDFInfo
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- CN105540640B CN105540640B CN201610051964.8A CN201610051964A CN105540640B CN 105540640 B CN105540640 B CN 105540640B CN 201610051964 A CN201610051964 A CN 201610051964A CN 105540640 B CN105540640 B CN 105540640B
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 84
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 27
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 4
- 239000005457 ice water Substances 0.000 claims abstract description 4
- 239000002244 precipitate Substances 0.000 claims abstract description 4
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000004246 zinc acetate Substances 0.000 claims abstract description 3
- RSWGJHLUYNHPMX-ONCXSQPRSA-N abietic acid Chemical compound C([C@@H]12)CC(C(C)C)=CC1=CC[C@@H]1[C@]2(C)CCC[C@@]1(C)C(O)=O RSWGJHLUYNHPMX-ONCXSQPRSA-N 0.000 claims description 17
- 238000005406 washing Methods 0.000 claims description 8
- DBJUEJCZPKMDPA-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O DBJUEJCZPKMDPA-UHFFFAOYSA-N 0.000 claims description 6
- 238000002425 crystallisation Methods 0.000 claims description 5
- 230000008025 crystallization Effects 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 3
- 238000001556 precipitation Methods 0.000 claims description 3
- 230000029087 digestion Effects 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 238000010792 warming Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 23
- 239000000047 product Substances 0.000 abstract description 8
- 230000001699 photocatalysis Effects 0.000 abstract description 4
- 238000001354 calcination Methods 0.000 abstract description 3
- 239000004094 surface-active agent Substances 0.000 abstract description 3
- 230000032683 aging Effects 0.000 abstract description 2
- 238000005516 engineering process Methods 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 abstract 2
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 abstract 2
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 abstract 2
- 238000000967 suction filtration Methods 0.000 abstract 1
- 230000015556 catabolic process Effects 0.000 description 12
- 238000006731 degradation reaction Methods 0.000 description 12
- 230000001476 alcoholic effect Effects 0.000 description 9
- 230000003197 catalytic effect Effects 0.000 description 7
- 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 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 6
- 229960000907 methylthioninium chloride Drugs 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 2
- 229960004756 ethanol Drugs 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 239000002073 nanorod Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000002574 poison Substances 0.000 description 2
- 231100000614 poison Toxicity 0.000 description 2
- -1 polytetrafluoroethylene Polymers 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 2
- 235000013904 zinc acetate Nutrition 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 150000001491 aromatic compounds Chemical class 0.000 description 1
- 239000000987 azo dye Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 229960000935 dehydrated alcohol Drugs 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229930014626 natural product Natural products 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- DJWUNCQRNNEAKC-UHFFFAOYSA-L zinc acetate Chemical class [Zn+2].CC([O-])=O.CC([O-])=O DJWUNCQRNNEAKC-UHFFFAOYSA-L 0.000 description 1
Classifications
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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
- B01J23/06—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- 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
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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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
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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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
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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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
- C01P2004/30—Particle morphology extending in three dimensions
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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
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Nanotechnology (AREA)
- Materials Engineering (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
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Abstract
The invention discloses a preparation method of flower-shaped nanometer zinc oxide and relates to a preparation method of nanometer zinc oxide. The preparation method aims at preparing the nanometer zinc oxide which is high in crystallinity and stability, large in specific surface area and free of clustering and has other characteristics. Rosin which is low in price and easy to obtain serves as surfactant to prepare the nanoscale zinc oxide. The method includes the following steps that an alcohol solution of rosin is added into a sodium hydroxide solution and is mixed evenly, and a zinc acetate solution is slowly added dropwise under the conditions of ice water bath and stirring; aging is performed at room temperature, then a hydrothermal reaction is performed, natural cooling and crystallizing are performed, suction filtration is performed, precipitate is washed, calcinating is performed after drying, and then the flower-shaped nanometer zinc oxide is obtained. The product obtained through the preparation method is free of clustering, large in specific surface area and high in photocatalytic activity, the hydrothermal synthesis method technology is simple, production cost is low, and industrial production can be achieved.
Description
Technical field
The invention belongs to the technical field of nano material；It is related to a kind of preparation method of nano zine oxide；Specifically related to one
Plant the preparation method with nano zine oxides of characteristic such as specific surface area are big, catalysis activity is high, stability is strong.
Background technology
With developing rapidly for modernization industry, the industrial wastewater containing organic poison is drained in the middle of environment in a large number, is caused
Make water resource heavily contaminated, threaten the survival and development of the mankind.It is particularly some azo dyes, polyhalohydrocarbon and nitre
Base aromatic compound, their Stability Analysis of Structures, strong toxicity, intractability are very big so that traditional environment project is effective very
It is micro-.Therefore, at present in the urgent need to finding new, more suitable effectively method of wastewater treatment making up the deficiency of conventional art.Half
The appearance of conductor metal oxide photocatalysis oxidation technique has brought hope, and it mainly includes TiO2、ZnO、WO3、
SnO2、Fe2O3Etc. N-type semiconductor material.Among these, TiO2Because of its stable chemical nature, oxidability is strong, the characteristic such as nontoxic and
Become most ripe, the most widely used nano photocatalyst catalytic material of research.However, with going deep into photocatalytic degradation organic poison
Research, it has been found that nano-ZnO compares TiO under many circumstances2Photocatalysis effect it is more preferable.With TiO2Compare, ZnO has following
Advantage：(1) larger range of ultraviolet light can be absorbed；(2)TiO2It is indirect band-gap semiconductor, electron transition probability is relatively low, amount
Son is less efficient, and catalytic reaction process is also slow, it is difficult to process the big waste water of those concentration height, quantity.Conversely, ZnO is direct band
, there are no these in gap semiconductor.(3) meet specific physics and chemistry while will keeping higher photocatalytic activity again
Can be difficult uniformly to be supported on other carriers which securely under conditions of requiring, and comparatively ZnO makes it easy to carry at other
Adsorb on body.So ZnO can replace TiO2Become more promising new catalyst.
At present, the preparation method of nanoscale ZnO can be divided mainly into three classes：Solid phase method, liquid phase method, vapor phase method.With other sides
Method is compared, and liquid phase method has that simple, reaction system is uniform, nanoparticle average particle size distribution is narrower, reaction temperature is low
The characteristics of, it is the prefered method for preparing excellent nano ZnO material.But, nano-ZnO is caused due to its huge surface energy
Grain is easy to reunite together so as to which pattern and size change, and have a strong impact on the performance of final products.Additionally, which is in purple
It also occur that serious photoetch under conditions of outer light irradiation.Therefore will solve the above problems, it is necessary to its preparation condition is carried out sternly
Lattice are controlled -- different surfactants is introduced in the preparation process of nano-ZnO be many scholars selections method.Therefore,
It is current problem demanding prompt solution to search out suitable surfactant, is to prepare that particle diameter is less, the more preferable nano-ZnO material of dispersibility
The key point of material.
The content of the invention
The invention discloses a kind of preparation method of flower-like nanometer Zinc Oxide；Purpose be prepare it is a kind of have high-crystallinity,
The nano zine oxide of the characteristics such as high stability, bigger serface, soilless sticking.
A kind of preparation method of flower-like nanometer Zinc Oxide of the present invention is carried out in the steps below：By the alcoholic solution of Colophonium
Be added in sodium hydroxide solution, mix homogeneously, then acetic acid zinc solution is slowly added dropwise under conditions of ice-water bath and stirring；Then
It is aged under room temperature, then carries out hydro-thermal reaction, natural cooling crystallization, sucking filtration, washing precipitation is calcined after drying, that is, obtain flower-shaped receiving
Rice Zinc Oxide.
Further limit：The mass concentration of the alcoholic solution of the Colophonium is 0.1～0.2g/mL, in the alcoholic solution of Colophonium
Alcohol is ethanol.The alcoholic solution of 10～20mL Colophonium is added to into the NaOH solution that 36～90mL concentration is 2～5mol/L, zinc acetate
Solution usage is 30～40mL, and the concentration of acetic acid zinc solution is 0.8～1.0mol/L.The drop speed of the acetic acid zinc solution is 1.5
～2mL/min.The digestion time is 2～3h.The hydro-thermal reaction is 5～12h of reaction under the conditions of 75 DEG C.It is described naturally cold
But crystallization time is 1～2h.Described washing precipitation is first with the deionized water again of absolute ethanol washing 2～3 times by precipitate
Washing 2～3 times.Dry under the conditions of 40～80 DEG C.Described calcining is with the intensification speed of 3～10 DEG C/min under air conditionses
Rate is heated to 205～300 DEG C, is incubated 1～3 hour, is further continued for being warming up to 500～650 DEG C, is incubated 1～3 hour.
Method of the present invention process is simple, equipment requirements be not high, and the low in raw material price such as Colophonium, ethanol is easy to get, Er Qieyi
In recovery, therefore low production cost, can large-scale industrial production.
The Colophonium that the inventive method is used is natural product, and environmental friendliness will not cause pollution.
The basic soilless sticking of nano granular of zinc oxide that the inventive method is obtained, good dispersion.
The flower-like nanometer Zinc Oxide that the inventive method is obtained is formed by a large amount of nanometer rods self assemblies, regular appearance, homogeneous, is put down
90 ran of equal particle diameter, specific surface area are big.
Understand that its diffraction maximum is very sharp by the XRD nanometers collection of illustrative plates of the flower-like nanometer Zinc Oxide of the present invention, illustrate degree of crystallinity very
Height, and there are not impurity peaks, illustrate that purity is very high.
The flower-like nanometer zinc oxide photocatalysis activity that the inventive method is obtained is high.With flower-shaped obtained in 0.1g the inventive method
Nano zine oxide catalytic degradation 100mL concentration under the irradiation of 18W uviol lamps is the methylene blue solution of 5mg/L, is persistently stirred
2.5h, degradation rate nearly 100%.
Description of the drawings
Fig. 1 is the electron scanning micrograph of one products obtained therefrom of specific embodiment.
Fig. 2 is the electron scanning micrograph that specific embodiment one does not add Colophonium products obtained therefrom.
Fig. 3 is the transmission electron microscope photo of three products obtained therefrom of specific embodiment.
Fig. 4 is the X-ray diffraction analysis figure of three products obtained therefrom of specific embodiment.
It is dense that Fig. 5 is that one～tetra- products obtained therefrom of specific embodiment takes 0.1g catalytic degradation 100mL under 18W ultra violet lamps
Spend the degradation rate of the methylene blue solution for 5mg/L；In Fig. 5, ■ represents specific embodiment one, ● represent specific embodiment
Two, ▲ specific embodiment three is represented, ▼ represents specific embodiment four.
Specific embodiment
Specific embodiment one：In present embodiment, the preparation method of flower-like nanometer Zinc Oxide is to carry out in the steps below
's：
10g Colophonium is dissolved in into 100mL dehydrated alcohol, the alcoholic solution of the Colophonium of 0.1g/mL is made.
5g zinc acetates are dissolved in 30mL deionized waters and obtain acetic acid zinc solution.
The alcoholic solution of 20mL Colophonium is added to into the hydrogen that 90mL concentration is that 2mol/L is configured with deionized water by sodium hydroxide
In sodium hydroxide solution, it is uniformly mixed, then acetic acid zinc solution is slowly added dropwise under conditions of ice-water bath and stirring, control drop speed
For 1.5mL/min；Then 2h is aged under room temperature, pours the high-pressure hydrothermal reaction kettle of inner liner polytetrafluoroethylene into, be placed in 75 DEG C of baking ovens
In carry out hydro-thermal reaction 12h, natural cooling crystallization 1h, sucking filtration, precipitate are first washed with deionized water for 3 times again with absolute ethanol washing
Wash 3 times, dry at 80 DEG C, be placed in sintering furnace and calcined, first programming rate is 10 DEG C/min, 1h is incubated at 300 DEG C, then
600 DEG C are continuously heating to, then are incubated 1h, that is, obtain flower-like nanometer Zinc Oxide.
From Fig. 1 and Fig. 2, the nano zine oxide prepared by Colophonium, a diameter of 10m of flowers, each oxidation are not added
Reunite between zinc bar heavier；The Zinc Oxide for adding Colophonium to prepare, its zinc oxide nano rod of flowers diameter on 5m, flowers are not rolled into a ball
Poly- phenomenon.It can be seen that the introducing of Colophonium substantially causes the pattern of Zinc Oxide to become regular orderly, the diameter of nanometer flowers diminishes.
With flower-like nanometer Zinc Oxide catalytic degradation under the irradiation of 18W uviol lamps obtained in 0.1g present embodiment methods
100mL concentration is the methylene blue solution of 5mg/L, persistently stirs 2.5h, degradation rate nearly 100% (referring to Fig. 5).
Specific embodiment two：Present embodiment from unlike specific embodiment one：By the alcoholic solution of 20mL Colophonium
It is added in the sodium hydroxide solution that 60mL concentration is 3mol/L.Other steps and parameter are identical with specific embodiment one.
With flower-like nanometer Zinc Oxide catalytic degradation under the irradiation of 18W uviol lamps obtained in 0.1g present embodiment methods
100mL concentration is the methylene blue solution of 5mg/L, persistently stirs 2.5h, degradation rate nearly 100% (referring to Fig. 5).
Specific embodiment three：Present embodiment from unlike specific embodiment one：By the alcoholic solution of 20mL Colophonium
It is added in the sodium hydroxide solution that 45mL concentration is 4mol/L.Other steps and parameter are identical with specific embodiment one.
As seen from Figure 3, the nanorod length formed by Zinc Oxide is 400 nanometers, and width is in 90 rans.
Product after calcining as seen from Figure 4 is pure Zinc Oxide, and without other impurity, degree of crystallinity is high.
With flower-like nanometer Zinc Oxide catalytic degradation under the irradiation of 18W uviol lamps obtained in 0.1g present embodiment methods
100mL concentration is the methylene blue solution of 5mg/L, persistently stirs 2.5h, degradation rate nearly 100% (referring to Fig. 5).
Specific embodiment four：Present embodiment from unlike specific embodiment one：By the alcoholic solution of 20mL Colophonium
It is added in the sodium hydroxide solution that 36mL concentration is 5mol/L.Other steps and parameter are identical with specific embodiment one.
With flower-like nanometer Zinc Oxide catalytic degradation under the irradiation of 18W uviol lamps obtained in 0.1g present embodiment methods
100mL concentration is the methylene blue solution of 5mg/L, persistently stirs 2.5h, degradation rate nearly 100% (referring to Fig. 5).
Specific embodiment five：Present embodiment from unlike specific embodiment one：Solution after ageing is poured into
The high-pressure hydrothermal reaction kettle of inner liner polytetrafluoroethylene, is placed in 5h in 75 DEG C of baking ovens.Other steps and parameter and specific embodiment
One is identical.
Claims (6)
1. a kind of preparation method of flower-like nanometer Zinc Oxide, it is characterised in that a kind of preparation method of flower-like nanometer Zinc Oxide be by
What following step was carried out：
Ethanol solution of 10 ~ 20mL mass concentrations for the Colophonium of 0.1 ~ 0.2g/mL is added to into 36 ~ 90mL concentration for 2 ~ 5mol/
In the sodium hydroxide solution of L, mix homogeneously, then be slowly added dropwise under conditions of ice-water bath and stirring 30 ~ 40mL concentration for 0.8 ~
The acetic acid zinc solution of 1.0mol/L；Then it is aged under room temperature, then 5 ~ 12 h of hydro-thermal reaction, natural cooling is carried out under the conditions of 75 DEG C
Crystallization, sucking filtration, washing precipitation under air conditionses are heated to 205 ~ 300 DEG C with the heating rate of 3 ~ 10 DEG C/min after drying, protect
Temperature 1 ~ 3 hour, is further continued for being warming up to 500 ~ 650 DEG C, is incubated 1 ~ 3 hour, that is, obtains flower-like nanometer Zinc Oxide.
2. the preparation method of a kind of flower-like nanometer Zinc Oxide according to claim 1, it is characterised in that the zinc acetate is molten
The drop speed of liquid is 1.5 ~ 2mL/min.
3. a kind of preparation method of flower-like nanometer Zinc Oxide according to claim 1, it is characterised in that the digestion time
For 2 ~ 3h.
4. a kind of preparation method of flower-like nanometer Zinc Oxide according to claim 1, it is characterised in that the natural cooling
Crystallization time is 1 ~ 2h.
5. the preparation method of a kind of flower-like nanometer Zinc Oxide according to claim 1, it is characterised in that described washing is sunk
Shallow lake is that first 2 ~ 3 times precipitate is washed with deionized 2 ~ 3 times again with absolute ethanol washing.
6. the preparation method of a kind of flower-like nanometer Zinc Oxide according to claim 1, it is characterised in that in 40 ~ 80 DEG C of conditions
Lower drying.
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| CN107128965A (en) * | 2017-05-31 | 2017-09-05 | 上海紫东薄膜材料股份有限公司 | A kind of preparation method of the nano zine oxide with barrier ultraviolet light and blue light |
| CN107737942B (en) * | 2017-10-23 | 2020-05-19 | 南京工程学院 | Zero-valent iron/flower-like zinc oxide nano composite material and preparation method thereof |
| CN108344793B (en) * | 2018-02-08 | 2023-08-25 | 浙江亿纳谱生命科技有限公司 | Matrix, preparation method thereof and mass spectrometry detection method of metabolic molecules |
| CN111392765A (en) * | 2020-05-08 | 2020-07-10 | 天津翔龙电子有限公司 | Process for preparing ZnO nano-particles by hydrothermal method |
| CN114084901B (en) * | 2021-11-25 | 2023-11-24 | 广州先护特农业科技有限公司 | Nano antibacterial material and preparation method and application thereof |
| CN114409923B (en) * | 2021-11-25 | 2023-10-20 | 华南农业大学 | Multifunctional self-healing antibacterial hydrogel and preparation method and application thereof |
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| CN104118903A (en) * | 2014-07-31 | 2014-10-29 | 济南大学 | Method for preparing three-dimensional flower-shaped zinc oxide nano material |
| CN104229864A (en) * | 2014-09-09 | 2014-12-24 | 上海纳米技术及应用国家工程研究中心有限公司 | Low-temperature preparation method of morphology-controllable zinc oxide nano materials |
| CN104445367A (en) * | 2014-11-13 | 2015-03-25 | 华侨大学 | Preparation method of nanoflower-shaped zinc oxide |
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| CN104118903A (en) * | 2014-07-31 | 2014-10-29 | 济南大学 | Method for preparing three-dimensional flower-shaped zinc oxide nano material |
| CN104229864A (en) * | 2014-09-09 | 2014-12-24 | 上海纳米技术及应用国家工程研究中心有限公司 | Low-temperature preparation method of morphology-controllable zinc oxide nano materials |
| CN104445367A (en) * | 2014-11-13 | 2015-03-25 | 华侨大学 | Preparation method of nanoflower-shaped zinc oxide |
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