CN112607763A - Method for controllably preparing multi-morphology micro-nano zinc oxide by hydrothermal method - Google Patents
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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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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 100
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 49
- 238000000034 method Methods 0.000 title claims abstract description 24
- 238000001027 hydrothermal synthesis Methods 0.000 title claims abstract description 16
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000008367 deionised water Substances 0.000 claims abstract description 11
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 11
- 239000002244 precipitate Substances 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 235000010299 hexamethylene tetramine Nutrition 0.000 claims abstract description 5
- 239000004312 hexamethylene tetramine Substances 0.000 claims abstract description 5
- YZYKBQUWMPUVEN-UHFFFAOYSA-N zafuleptine Chemical compound OC(=O)CCCCCC(C(C)C)NCC1=CC=C(F)C=C1 YZYKBQUWMPUVEN-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000002243 precursor Substances 0.000 claims abstract description 3
- 239000012456 homogeneous solution Substances 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000000047 product Substances 0.000 abstract description 9
- 244000288784 Posoqueria latifolia Species 0.000 abstract description 4
- 238000003756 stirring Methods 0.000 abstract description 2
- 230000001276 controlling effect Effects 0.000 abstract 1
- 238000001816 cooling Methods 0.000 abstract 1
- 238000011049 filling Methods 0.000 abstract 1
- 238000007172 homogeneous catalysis Methods 0.000 abstract 1
- 239000000843 powder Substances 0.000 abstract 1
- 230000001105 regulatory effect Effects 0.000 abstract 1
- 238000001308 synthesis method Methods 0.000 abstract 1
- 238000005303 weighing Methods 0.000 abstract 1
- 238000002360 preparation method Methods 0.000 description 12
- 239000002245 particle Substances 0.000 description 5
- 239000004809 Teflon Substances 0.000 description 4
- 229920006362 Teflon® Polymers 0.000 description 4
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 230000006750 UV protection Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000005018 casein Substances 0.000 description 1
- BECPQYXYKAMYBN-UHFFFAOYSA-N casein, tech. Chemical compound NCCCCC(C(O)=O)N=C(O)C(CC(O)=O)N=C(O)C(CCC(O)=N)N=C(O)C(CC(C)C)N=C(O)C(CCC(O)=O)N=C(O)C(CC(O)=O)N=C(O)C(CCC(O)=O)N=C(O)C(C(C)O)N=C(O)C(CCC(O)=N)N=C(O)C(CCC(O)=N)N=C(O)C(CCC(O)=N)N=C(O)C(CCC(O)=O)N=C(O)C(CCC(O)=O)N=C(O)C(COP(O)(O)=O)N=C(O)C(CCC(O)=N)N=C(O)C(N)CC1=CC=CC=C1 BECPQYXYKAMYBN-UHFFFAOYSA-N 0.000 description 1
- 235000021240 caseins Nutrition 0.000 description 1
- -1 catalysis Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000001451 molecular beam epitaxy Methods 0.000 description 1
- 239000002073 nanorod Substances 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 150000003751 zinc Chemical class 0.000 description 1
- 239000011701 zinc 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
- B01J23/06—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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- 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
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a method for controllably preparing multi-morphology micro-nano zinc oxide by a hydrothermal method, which comprises the following steps: weighing zinc acetate dihydrate and hexamethylenetetramine in equal proportion, putting the zinc acetate dihydrate and the hexamethylenetetramine into a beaker, adding deionized water, stirring, transferring the solution into an autoclave, reacting at 90-100 ℃, cooling the autoclave to room temperature, collecting white precipitate, filtering the white precipitate for several times by using the deionized water, drying an obtained sample, putting an obtained precursor into a muffle furnace for roasting, and filling powder obtained after roasting into a sample bag. The invention provides a method for preparing zinc oxide with multiple morphologies in a controllable manner based on a hydrothermal method, and zinc oxide with multiple morphologies such as hexagonal discs, screw caps, needle flowers, swords and the like is prepared by regulating and controlling the concentration of a solution. The obtained product has controllable granularity, better uniformity, low cost and simple synthesis method. The obtained product has better stability and can be widely applied to 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 | Preparation method of zinc oxide modified fabric with dual functions of ultraviolet resistance and adsorptivity |
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