CN105540640A - Preparation method of flower-shaped nanometer zinc oxide - Google Patents
Preparation method of flower-shaped nanometer zinc oxide Download PDFInfo
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- CN105540640A CN105540640A CN201610051964.8A CN201610051964A CN105540640A CN 105540640 A CN105540640 A CN 105540640A CN 201610051964 A CN201610051964 A CN 201610051964A CN 105540640 A CN105540640 A CN 105540640A
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 95
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 30
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 claims abstract description 22
- 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 claims abstract description 22
- 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 claims abstract description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 9
- 238000001354 calcination Methods 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 230000032683 aging Effects 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
- 238000003756 stirring Methods 0.000 claims abstract description 4
- 238000000967 suction filtration Methods 0.000 claims abstract description 4
- 230000001476 alcoholic effect Effects 0.000 claims description 13
- DBJUEJCZPKMDPA-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O DBJUEJCZPKMDPA-UHFFFAOYSA-N 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000002425 crystallisation Methods 0.000 claims description 5
- 230000008025 crystallization Effects 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000001556 precipitation Methods 0.000 claims description 4
- 238000010792 warming Methods 0.000 claims description 3
- 230000029087 digestion Effects 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 23
- 239000000047 product Substances 0.000 abstract description 8
- 230000001699 photocatalysis Effects 0.000 abstract description 4
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 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
- 239000004246 zinc acetate Substances 0.000 abstract description 2
- 239000002244 precipitate Substances 0.000 abstract 1
- 239000004094 surface-active agent Substances 0.000 abstract 1
- 230000015556 catabolic process Effects 0.000 description 12
- 238000006731 degradation reaction Methods 0.000 description 12
- 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
- 229910010413 TiO 2 Inorganic materials 0.000 description 6
- 229960000907 methylthioninium chloride Drugs 0.000 description 6
- 238000013019 agitation Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- -1 WO 3 Inorganic materials 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 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
- 239000013543 active substance Substances 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000000694 effects Effects 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
- 239000002574 poison Substances 0.000 description 2
- 231100000614 poison Toxicity 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 229910006404 SnO 2 Inorganic materials 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
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000011109 contamination Methods 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
- 238000009826 distribution Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 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
- 238000006862 quantum yield reaction Methods 0.000 description 1
- 239000002994 raw material Substances 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
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000009281 ultraviolet germicidal irradiation Methods 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
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 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
-
- B01J35/39—
-
- 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
-
- 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
-
- 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
-
- 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
-
- 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
-
- 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
-
- 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
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; Relate to a kind of preparation method of nano zine oxide; Be specifically related to a kind of preparation method with the nano zine oxide of the characteristics such as specific surface area is large, catalytic activity is high, stability is strong.
Background technology
Along with developing rapidly of modernization industry, a large amount of trade effluent containing organic poison is drained in the middle of environment, causes water resources to be subject to severe contamination, has threatened the survival and development of the mankind.Particularly some azoic dyestuffs, polyhalohydrocarbon and nitro-aromatic compound, their Stability Analysis of Structures, strong toxicity, intractability is very large, makes traditional environment project effective very micro-.Therefore, at present in the urgent need to finding new, more suitable effective method of wastewater treatment to make up the deficiency of conventional art.The appearance of metal oxide semiconductor photocatalysis oxidation technique has brought hope, and it mainly comprises TiO
2, ZnO, WO
3, SnO
2, Fe
2o
3deng N-type semiconductor material.This wherein, TiO
2because of its stable chemical nature, characteristics such as oxidation capacity is strong, nontoxic and become the most ripe, the most widely used nano photocatalyst catalytic material of research.But, along with the further investigation to photocatalytic degradation organic poison, it is found that nano-ZnO under many circumstances than TiO
2photocatalysis effect better.With TiO
2compare, ZnO has following advantage: (1) can absorb wider UV-light; (2) TiO
2be indirect band-gap semiconductor, transition of electron probability is lower, and quantum yield is lower, and catalyzed reaction process is also slow, is difficult to process the waste water that those concentration are high, quantity is large.On the contrary, ZnO is direct band-gap semicondictor, there is not these problems.(3) be difficult to it meet the condition that specific physicochemical property requires again while will keeping higher photocatalytic activity under that evenly load is on other carrier securely, and ZnO is just easy to adsorb on other carrier comparatively speaking.So ZnO can replace TiO
2become more promising new catalyst.
At present, the preparation method of nano level ZnO mainly can be divided three classes: solid phase method, liquid phase method, vapor phase process.Compared with other method, liquid phase method have simple, reaction system evenly, the feature that average particle size distribution is narrower, temperature of reaction is low of nanoparticle, be the prefered method preparing excellent nano ZnO material.But nano-ZnO, due to its huge surface energy, causes particle to be easy to reunite together, makes its pattern and size change, have a strong impact on the performance of the finished product.In addition, also can there is serious photoetch in it under the condition of UV-irradiation.Therefore will solve the problem, strictly must control its preparation condition--being introduced by different tensio-active agents in the preparation process of nano-ZnO is the method that a lot of scholar selects.Therefore, finding out suitable tensio-active agent is current problem demanding prompt solution, is the key point preparing less, the dispersed better nano ZnO material of particle diameter.
Summary of the invention
The invention discloses a kind of preparation method of flower-like nanometer zinc oxide; Object is a kind of nano zine oxide with characteristics such as high-crystallinity, high stability, bigger serface, soilless sticking of preparation.
The preparation method of a kind of flower-like nanometer zinc oxide of the present invention carries out in the steps below: join in sodium hydroxide solution by the alcoholic solution of rosin, mix, more slowly drips acetic acid zinc solution under the condition of ice-water bath and stirring; Then ageing under room temperature, then carry out hydro-thermal reaction, natural cooling crystallization, suction filtration, washing precipitation, after drying, calcining, namely obtains flower-like nanometer zinc oxide.
Further restriction: the mass concentration of the alcoholic solution of described rosin is 0.1 ~ 0.2g/mL, and the alcohol in the alcoholic solution of rosin is ethanol.The alcoholic solution of 10 ~ 20mL rosin is joined the NaOH solution that 36 ~ 90mL concentration is 2 ~ 5mol/L, and acetic acid zinc solution consumption is 30 ~ 40mL, and the concentration of acetic acid zinc solution is 0.8 ~ 1.0mol/L.A speed of described acetic acid zinc solution is 1.5 ~ 2mL/min.Described digestion time is 2 ~ 3h.Described hydro-thermal reaction reacts 5 ~ 12h under 75 DEG C of conditions.The described natural cooling crystallization time is 1 ~ 2h.Described washing precipitation is that throw out is first used deionized water wash 2 ~ 3 times for 2 ~ 3 times again with absolute ethanol washing.Dry under 40 ~ 80 DEG C of conditions.Described calcining is heated to 205 ~ 300 DEG C with the temperature rise rate of 3 ~ 10 DEG C/min under air conditions, is incubated 1 ~ 3 hour, then continues to be warming up to 500 ~ 650 DEG C, is incubated 1 ~ 3 hour.
Method technique of the present invention is simple, and equipment requirements is not high, and the low in raw material price such as rosin, ethanol is easy to get, and is easy to reclaim, therefore production cost is low, can large-scale industrial production.
The rosin that the inventive method uses is natural product, and environmental friendliness, can not cause pollution.
The basic soilless sticking of nano granular of zinc oxide that the inventive method obtains, good dispersity.
The flower-like nanometer zinc oxide that the inventive method obtains is formed by a large amount of nanometer rod self-assembly, regular appearance, homogeneous, and median size 90 ran, specific surface area is large.
Very sharp-pointed by XRD nanometer collection of illustrative plates its diffraction peak known of flower-like nanometer zinc oxide of the present invention, illustrate that degree of crystallinity is very high, and do not occur impurity peaks, illustrate that purity is very high.
The flower-like nanometer zinc oxide photocatalysis activity that the inventive method obtains is high.The flower-like nanometer zinc oxide obtained by 0.1g the inventive method catalyzed degradation 100mL concentration under the irradiation of 18W ultraviolet lamp is the methylene blue solution of 5mg/L, Keep agitation 2.5h, degradation rate nearly 100%.
Accompanying drawing explanation
Fig. 1 is the electron scanning micrograph of embodiment one products obtained therefrom.
Fig. 2 is the electron scanning micrograph that embodiment one does not add rosin products obtained therefrom.
Fig. 3 is the transmission electron microscope photo of embodiment three products obtained therefrom.
Fig. 4 is the X-ray diffraction analysis figure of embodiment three products obtained therefrom.
Fig. 5 is that to get 0.1g catalyzed degradation 100mL concentration under 18W ultra violet lamp be the degradation rate of the methylene blue solution of 5mg/L to embodiment one ~ tetra-products obtained therefrom; In Fig. 5, ■ represents embodiment one, ● represent embodiment two, ▲ represent that embodiment three, ▼ represents embodiment four.
Embodiment
Embodiment one: in present embodiment, the preparation method of flower-like nanometer zinc oxide carries out in the steps below:
10g rosin is dissolved in 100mL dehydrated alcohol, makes the alcoholic solution of the rosin of 0.1g/mL.
5g zinc acetate is dissolved in 30mL deionized water and obtains acetic acid zinc solution.
The alcoholic solution of 20mL rosin being joined 90mL concentration is in the sodium hydroxide solution that configured by sodium hydroxide and deionized water of 2mol/L, is uniformly mixed, more slowly drips acetic acid zinc solution under the condition of ice-water bath and stirring, and controlling to drip speed is 1.5mL/min; Then ageing 2h under room temperature, pours the high-pressure hydrothermal reaction kettle of inner liner polytetrafluoroethylene into, is placed in 75 DEG C of baking ovens and carries out hydro-thermal reaction 12h, natural cooling crystallization 1h, suction filtration, throw out first uses deionized water wash 3 times for 3 times again with absolute ethanol washing, dries at 80 DEG C, be placed in sintering oven to calcine, first heat-up rate is 10 DEG C/min, at 300 DEG C of insulation 1h, then continues to be warming up to 600 DEG C, be incubated 1h again, namely obtain flower-like nanometer zinc oxide.
From Fig. 1 and Fig. 2, do not add the nano zine oxide prepared by rosin, flowers diameter is 10m, reunites heavier between each oxidation zinc bar; Add zinc oxide prepared by rosin, its flowers diameter is at 5m, and the zinc oxide nano rod on flowers does not have agglomeration.The introducing of visible rosin obviously makes the pattern of zinc oxide become in order regular, and the diameter of nanometer flowers diminishes.
The flower-like nanometer zinc oxide obtained by 0.1g present embodiment method catalyzed degradation 100mL concentration under the irradiation of 18W ultraviolet lamp is the methylene blue solution of 5mg/L, and Keep agitation 2.5h, degradation rate is 100% (see Fig. 5) nearly.
Embodiment two: present embodiment and embodiment one unlike: the alcoholic solution of 20mL rosin being joined 60mL concentration is in the sodium hydroxide solution of 3mol/L.Other step is identical with embodiment one with parameter.
The flower-like nanometer zinc oxide obtained by 0.1g present embodiment method catalyzed degradation 100mL concentration under the irradiation of 18W ultraviolet lamp is the methylene blue solution of 5mg/L, and Keep agitation 2.5h, degradation rate is 100% (see Fig. 5) nearly.
Embodiment three: present embodiment and embodiment one unlike: the alcoholic solution of 20mL rosin being joined 45mL concentration is in the sodium hydroxide solution of 4mol/L.Other step is identical with embodiment one with parameter.
As seen from Figure 3, zinc oxide formed nanorod length be 400 nanometers, width is at 90 ran.
Product as seen from Figure 4 after calcining is pure zinc oxide, and not containing other impurity, degree of crystallinity is high.
The flower-like nanometer zinc oxide obtained by 0.1g present embodiment method catalyzed degradation 100mL concentration under the irradiation of 18W ultraviolet lamp is the methylene blue solution of 5mg/L, and Keep agitation 2.5h, degradation rate is 100% (see Fig. 5) nearly.
Embodiment four: present embodiment and embodiment one unlike: the alcoholic solution of 20mL rosin being joined 36mL concentration is in the sodium hydroxide solution of 5mol/L.Other step is identical with embodiment one with parameter.
The flower-like nanometer zinc oxide obtained by 0.1g present embodiment method catalyzed degradation 100mL concentration under the irradiation of 18W ultraviolet lamp is the methylene blue solution of 5mg/L, and Keep agitation 2.5h, degradation rate is 100% (see Fig. 5) nearly.
Embodiment five: present embodiment and embodiment one unlike: the high-pressure hydrothermal reaction kettle solution after ageing being poured into inner liner polytetrafluoroethylene, is placed in 75 DEG C of baking oven 5h.Other step is identical with embodiment one with parameter.
Claims (10)
1. a preparation method for flower-like nanometer zinc oxide, is characterized in that a kind of preparation method of flower-like nanometer zinc oxide carries out in the steps below:
The alcoholic solution of rosin is joined in sodium hydroxide solution, mixes, more slowly drip acetic acid zinc solution under the condition of ice-water bath and stirring; Then ageing under room temperature, then carry out hydro-thermal reaction, natural cooling crystallization, suction filtration, washing precipitation, after drying, calcining, namely 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 characterized in that the mass concentration of the alcoholic solution of described rosin is 0.1 ~ 0.2g/mL, the alcohol in the alcoholic solution of rosin is ethanol.
3. the preparation method of a kind of flower-like nanometer zinc oxide according to claim 2, it is characterized in that the alcoholic solution of 10 ~ 20mL rosin to join the NaOH solution that 36 ~ 90mL concentration is 2 ~ 5mol/L, acetic acid zinc solution consumption is
30 ~ 40mL, the concentration of acetic acid zinc solution is 0.8 ~ 1.0mol/L.
4. the preparation method of a kind of flower-like nanometer zinc oxide according to claim 1, is characterized in that a speed of described acetic acid zinc solution is 1.5 ~ 2mL/min.
5. the preparation method of a kind of flower-like nanometer zinc oxide according to claim 1, is characterized in that described digestion time is 2 ~ 3h.
6. the preparation method of a kind of flower-like nanometer zinc oxide according to claim 1, is characterized in that described hydro-thermal reaction reacts 5 ~ 12h under 75 DEG C of conditions.
7. the preparation method of a kind of flower-like nanometer zinc oxide according to claim 1, is characterized in that the described natural cooling crystallization time is 1 ~ 2h.
8. the preparation method of a kind of flower-like nanometer zinc oxide according to claim 1, is characterized in that described washing precipitation is that throw out is first used deionized water wash 2 ~ 3 times for 2 ~ 3 times again with absolute ethanol washing.
9. the preparation method of a kind of flower-like nanometer zinc oxide according to claim 1, is characterized in that drying under 40 ~ 80 DEG C of conditions.
10. the preparation method of a kind of flower-like nanometer zinc oxide according to claim 1, it is characterized in that described calcining is heated to 205 ~ 300 DEG C with the temperature rise rate of 3 ~ 10 DEG C/min under air conditions, be incubated 1 ~ 3 hour, then continue to be warming up to 500 ~ 650 DEG C, be incubated 1 ~ 3 hour.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107029696A (en) * | 2017-05-12 | 2017-08-11 | 济南大学 | A kind of method that use green solvent prepares zinc oxide mesopore material at room temperature |
| 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 |
| CN107737942A (en) * | 2017-10-23 | 2018-02-27 | 南京工程学院 | A kind of Zero-valent Iron/flower shape zinc oxide nano composite material and preparation method thereof |
| CN108344793A (en) * | 2018-02-08 | 2018-07-31 | 亿纳谱（天津）医学检验中心有限公司 | A kind of matrix and preparation method thereof, the mass spectral analysis detection method of metabolic molecule |
| 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 |
| CN114084901A (en) * | 2021-11-25 | 2022-02-25 | 广州先护特农业科技有限公司 | Nano antibacterial material and preparation method and application thereof |
| CN114409923A (en) * | 2021-11-25 | 2022-04-29 | 华南农业大学 | Multifunctional self-healing antibacterial hydrogel and preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
-
2016
- 2016-01-26 CN CN201610051964.8A patent/CN105540640B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Non-Patent Citations (2)
| Title |
|---|
| 余方丹: "木质素基两性表面活性剂对ZnO纳米晶控制制备", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
| 陈素文: "《松香松节油深度加工技术与利用》", 31 January 1997 * |
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