CN112607763A - Method for controllably preparing multi-morphology micro-nano zinc oxide by hydrothermal method - Google Patents
Method for controllably preparing multi-morphology micro-nano zinc oxide by hydrothermal method Download PDFInfo
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- CN112607763A CN112607763A CN202110009809.0A CN202110009809A CN112607763A CN 112607763 A CN112607763 A CN 112607763A CN 202110009809 A CN202110009809 A CN 202110009809A CN 112607763 A CN112607763 A CN 112607763A
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- C01G9/00—Compounds of zinc
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
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Abstract
本发明公开一种水热法可控制备多形貌微纳米氧化锌的方法，所述方法包括如下步骤：称取等比例二水合乙酸锌和六亚甲基四胺放入烧杯中，加入去离子水并搅拌，然后将溶液转移到高压釜中并在90℃‑100℃下进行反应，等高压釜冷却至室温后收集白色沉淀，并用去离子水过滤数次，将所得样品进行干燥，然后将所得前驱体置于马弗炉中焙烧，把焙烧后所得粉末装入样品袋中。本发明基于水热法提出一种可控制备多形貌氧化锌的方法，通过对溶液浓度的调控，制备了六方盘状、螺帽状、针花状及剑状等多形貌的氧化锌。获得的产物粒度可控，均一性较好，且成本低廉，合成方法简单。所得产品具有较好的稳定性，可广泛应用于均相催化领域。
The invention discloses a method for the controllable preparation of multi-morphological micro-nano zinc oxide by a hydrothermal method. The method comprises the following steps: weighing equal proportions of zinc acetate dihydrate and hexamethylenetetramine into a beaker, adding ionized water and stirring, then transfer the solution to the autoclave and react at 90℃-100℃, collect the white precipitate after the autoclave is cooled to room temperature, filter with deionized water for several times, and dry the obtained sample, then The obtained precursor was calcined in a muffle furnace, and the powder obtained after calcination was placed in a sample bag. The invention proposes a method for controllable preparation of multi-morphological zinc oxide based on a hydrothermal method. By controlling the concentration of the solution, zinc oxide with multi-morphological hexagonal disk shape, nut shape, needle flower shape and sword shape is prepared. . The obtained product has controllable particle size, good uniformity, low cost and simple synthesis method. The obtained product has good stability and can be widely used in the field of homogeneous catalysis.
Description
Technical Field
The invention relates to a method for controllably preparing multi-morphology micro-nano zinc oxide by a hydrothermal method, belonging to the technical field of material preparation.
Background
Zinc oxide is a group II-VI semiconductor material, and has many special properties such as gas-sensitive property, photocatalytic property, antibacterial property, conductivity, and ultraviolet resistance due to the characteristics of fine crystal grains, and is widely used in the fields of chemical industry, textile, catalysis, cosmetics, medical and health, and the like. Researches show that the zinc oxide micro-nano materials obtained by different preparation methods have larger differences in morphology and microstructure, and further influence the physical and chemical properties and other application performances of zinc oxide, so that the controllable preparation of the zinc oxide micro-nano structure materials is favored by vast researchers.
At present, the preparation methods of zinc oxide (rod-shaped, spherical, flower-shaped, nanowire and the like) with different shapes mainly comprise a gas phase method and a liquid phase method. The vapor phase method mainly comprises Metal Organic Chemical Vapor Deposition (MOCVD), Molecular Beam Epitaxy (MBE), radio frequency magnetron sputtering, Pulse Laser Deposition (PLD) and the like, and the method has complex synthesis conditions, needs high vacuum and high temperature, and has expensive equipment, large energy consumption, higher cost and difficult industrialization. Therefore, compared with a gas phase method, the liquid phase method has the advantages of lower production cost, simpler condition requirement and wider application. The liquid phase method mainly comprises a micro-emulsion method, a sol-gel method, a hydrothermal method, a super-gravity method and a precipitation method. The product obtained by the hydrothermal method has the advantages of easier control of the particle size and better uniformity, and is widely applied to the preparation of various nano materials.
The preparation method comprises the following steps of firstly preparing a zinc oxide seed layer on a glass substrate by using a spin coating method, and then growing a zinc oxide nanorod array under different conditions by using a hydrothermal reaction; the patent [ CN 201210056193.3] takes casein as a template agent, takes zinc salt and ammonia water as raw materials, and obtains the micron-sphere zinc oxide by a hydrothermal method; guo Tengchao et al (Journal of Alloys and Compounds, 2019, 804, 503-. The method needs substrate growth or additive, and has the defects of high reaction requirement, complex equipment and the like, but the method can control the zinc oxide with rich appearance by controlling the concentration of the homogeneous solution under the same equipment and reaction condition, is simple and feasible, and the obtained zinc oxide has rich appearance, thereby being more beneficial to large-scale production and application.
Disclosure of Invention
The invention aims to provide various hydrothermal method controllable preparation methods of multi-morphology micro-nano zinc oxide, which can conveniently realize zinc oxide with different morphologies such as hexagonal disc shape, nut shape, needle shape and sword shape by the same equipment.
In order to achieve the aim, the invention provides a method for controllably preparing multi-morphology micro-nano zinc oxide by a hydrothermal method, which is characterized by comprising the following steps:
(1) dissolving zinc acetate dihydrate and hexamethylenetetramine in deionized water according to the molar weight ratio of 1:1 to obtain a homogeneous solution, wherein the concentration of the homogeneous solution is 0.01-0.12 mol/L
(2) Transferring the solution into an autoclave for reaction, and filtering the obtained white precipitate for several times by using deionized water after the autoclave is cooled after the reaction is finished;
(3) drying the obtained sample, placing the dried precursor in a muffle furnace for roasting, and obtaining zinc oxide powder after roasting is finished;
furthermore, the reaction temperature in the step (2) of the invention is 75-100 ℃, and the reaction time is 10-48 h.
Furthermore, in the step (3), the drying temperature is 60-80 ℃, and the drying time is 10-24 h.
Furthermore, in the step (3), the roasting temperature is 250-550 ℃, and the roasting time is 1-5 h.
The invention has the following beneficial effects:
the product obtained by the hydrothermal method has the advantages of easier control of the particle size, better uniformity, low cost and simple condition requirement.
According to the invention, different shapes of zinc oxide hexagonal discs, needle flowers and sword shapes are obtained by controlling the concentration of the solution, the change condition is very simple, the obtained shapes are rich, and the operation is convenient.
The zinc oxide obtained by the method has good hydrothermal stability, can be used as a catalyst or a carrier in the field of catalysis, improves the catalytic performance of the catalyst, and has great application potential in the field of catalysis.
Drawings
Fig. 1 is an SEM photograph of zinc oxide prepared in example 1.
Fig. 2 is an SEM photograph of zinc oxide prepared in example 2.
Fig. 3 is an SEM photograph of zinc oxide prepared in example 3.
Fig. 4 is an SEM photograph of zinc oxide prepared in example 3.
Fig. 1-4 are SEM photographs of hexagonal disks, nuts, needles, and swords, respectively, of zinc oxide.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to examples, but those skilled in the art will appreciate that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention.
The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products commercially available.
Example 1
A preparation method of hexagonal disk-shaped zinc oxide specifically comprises the following steps:
an equimolar amount of zinc acetate dihydrate (ZnAc)2，Zn(CO2CH3)2·2H2O) and hexamethylenetetramine (HMT, C)6H12N4) Put into a 500mL beaker (4.51g ZnAc)2And 2.88g HMT); adding 180ml of deionized water and stirring for 10min to fully dissolve the reagents to obtain a solution (denoted as solution A), then transferring the solution to a 500ml-Teflon lined autoclave and maintaining at 97 ℃ for 12 h; after the autoclave is cooled to room temperature, collecting white precipitate, and filtering the white precipitate for a plurality of times by using deionized water; all samples were dried at 60 ℃ for 12h and then calcined at 450 ℃ for 2 h; the obtained zinc oxide is shown in figure 1; as can be seen from the figure, the obtained product was a hexagonal disk-shaped zinc oxide having a hexagonal edge length of about 4 μm and a height of about 7.4. mu.m.
Example 2
A preparation method of nut-shaped zinc oxide specifically comprises the following steps:
the solution A in (1) was diluted 2-fold and then transferred to a 500ml-Teflon lined autoclave and held at 97 ℃ for 12 h; after the autoclave is cooled to room temperature, collecting white precipitate, and filtering the white precipitate for a plurality of times by using deionized water; all samples were dried at 60 ℃ for 12h and then calcined at 450 ℃ for 2 h; the obtained zinc oxide is shown in figure 2; as can be seen, the obtained product is nut-shaped zinc oxide, has uniform appearance and is formed by stacking nut shapes with different sizes.
Example 3
A preparation method of the needle-flower-shaped zinc oxide specifically comprises the following steps:
the solution A in (1) was diluted 7-fold and then transferred to a 500ml-Teflon lined autoclave and kept at 97 ℃ for 12 h; after the autoclave is cooled to room temperature, collecting white precipitate, and filtering the white precipitate for a plurality of times by using deionized water; all samples were dried at 60 ℃ for 12h and then calcined at 450 ℃ for 2 h; the obtained zinc oxide is shown in figure 3; as can be seen from the figure, the obtained product shows a kind of needle-flower-shaped zinc oxide, a small part of which is columnar and shows a tendency of converting to needle-flower shape.
Example 4
A preparation method of sword-shaped zinc oxide specifically comprises the following steps:
the solution A in (1) was diluted 12 times and then transferred to a 500ml Teflon lined autoclave and held at 97 ℃ for 12 h. After the autoclave was cooled to room temperature, a white precipitate was collected and filtered several times with deionized water. All samples were dried at 60 ℃ for 12h and then calcined at 450 ℃ for 2 h. The resulting zinc oxide is shown in fig. 4. As can be seen, the resulting product is a zinc oxide in the form of a sword, having a length of about 10 μm.
Experiments prove that the method sequentially realizes the preparation of hexagonal disc-shaped, needle-flower-shaped and sword-shaped zinc oxide by changing the concentration of zinc ions in the solution through the same method and equipment, namely, when the concentration of the homogeneous solution is about 0.12mol/L, the obtained zinc oxide is hexagonal disc-shaped; when the concentration of the homogeneous solution is about 0.06mol/L, the obtained zinc oxide is in a nut shape; when the concentration of the homogeneous solution is about 0.017mol/L, the obtained zinc oxide is in a needle flower shape; when the concentration of the homogeneous solution is about 0.01mol/L, the obtained zinc oxide is sword-shaped.
The specific form of zinc oxide is shown in fig. 1, fig. 2 and fig. 3, namely, when the concentration of zinc ions changes from high to low, the zinc oxide is from 0.12mol/L to 0.01mol/L, and the appearance of the zinc oxide gradually develops into a sword-shaped structure from a hexagonal disc-shaped structure with large specific surface area; therefore, the invention can conveniently prepare particles with better particle size, dispersibility and appropriateness by using the same method and equipment and changing the control of the concentration of zinc ions in the solution, and simultaneously realizes the complex and multi-shape of the particles so as to meet different application requirements.
Although the present invention has been described with reference to the preferred embodiments, it should be understood that various changes and modifications can be made therein by those skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (4)
1. A method for controllably preparing multi-morphology micro-nano zinc oxide by a hydrothermal method is characterized by comprising the following steps:
(1) dissolving zinc acetate dihydrate and hexamethylenetetramine in deionized water according to the molar weight ratio of 1:1 to obtain a homogeneous solution, wherein the concentration of the homogeneous solution is 0.01-0.12 mol/L
(2) Transferring the solution into an autoclave for reaction, and filtering the obtained white precipitate for several times by using deionized water after the autoclave is cooled after the reaction is finished;
(3) and drying the obtained sample, placing the dried precursor in a muffle furnace for roasting, and obtaining zinc oxide powder after roasting is finished.
2. The hydrothermal method of claim 1, wherein the method comprises the following steps: the reaction temperature in the step (2) is 75-100 ℃, and the reaction time is 10-48 h.
3. The hydrothermal method for controllably preparing the multi-morphology micro-nano zinc oxide according to claim 1, wherein in the step (3), the drying temperature is 60-80 ℃, and the drying time is 10-24 h.
4. The hydrothermal method for controllably preparing the multi-morphology micro-nano zinc oxide according to claim 1, wherein in the step (3), the roasting temperature is 250-550 ℃, and the roasting time is 1-5 h.
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Cited By (3)
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| CN113184895A (en) * | 2021-04-23 | 2021-07-30 | 西安交通大学 | Controllable double-layer prismatic-disk-shaped micron zinc oxide and preparation method thereof |
| CN113952917A (en) * | 2021-10-18 | 2022-01-21 | 济源市鲁泰纳米材料有限公司 | Hypergravity reactor and preparation method of active nano zinc oxide prepared by same |
| CN114108307A (en) * | 2021-11-02 | 2022-03-01 | 盐城工学院 | A kind of preparation method of zinc oxide modified fabric with dual functions of anti-ultraviolet and adsorption |
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Cited By (3)
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| CN113184895A (en) * | 2021-04-23 | 2021-07-30 | 西安交通大学 | Controllable double-layer prismatic-disk-shaped micron zinc oxide and preparation method thereof |
| CN113952917A (en) * | 2021-10-18 | 2022-01-21 | 济源市鲁泰纳米材料有限公司 | Hypergravity reactor and preparation method of active nano zinc oxide prepared by same |
| CN114108307A (en) * | 2021-11-02 | 2022-03-01 | 盐城工学院 | A kind of preparation method of zinc oxide modified fabric with dual functions of anti-ultraviolet and adsorption |
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Application publication date: 20210406 |