CN115072765B - Method for preparing hexagonal prism-shaped zinc oxide - Google Patents
Method for preparing hexagonal prism-shaped zinc oxide Download PDFInfo
- Publication number
- CN115072765B CN115072765B CN202210710924.5A CN202210710924A CN115072765B CN 115072765 B CN115072765 B CN 115072765B CN 202210710924 A CN202210710924 A CN 202210710924A CN 115072765 B CN115072765 B CN 115072765B
- Authority
- CN
- China
- Prior art keywords
- magnesium
- zinc oxide
- hydrothermal reaction
- hexagonal
- sodium hydroxide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- 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
-
- 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
- C01P2004/60—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
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention belongs to the technical field of chemical synthesis, and particularly relates to a method for preparing hexagonal prism-shaped zinc oxide. The invention reacts magnesium ions with sodium hydroxide to generate hexagonal flake Mg (OH) through substitution reaction 2 Crystals, then subjecting the obtained hexagonal columnar crystals Mg (OH) 2 With zinc salt, because the stability constant of zinc hydroxide is higher than that of magnesium hydroxide, zn 2+ Will take Mg (OH) 2 Hydroxyl ions in the crystal grow along a (0001) crystal face by taking the hydroxyl ions as a template to generate Zn (OH) 2 The hexagonal prism-shaped zinc oxide with uniform morphology is generated through hydrothermal reaction.
Description
Technical Field
The invention belongs to the technical field of chemical synthesis, and particularly relates to a method for preparing hexagonal prism-shaped zinc oxide.
Background
Increasingly global warming and environmental problems have caused researchers to continually seek more environmentally friendly and energy efficient techniques. Photocatalytic oxidation technology is an environmental remediation technology that utilizes semiconductor photocatalysts to degrade organic pollutants, and has been recognized as a more viable technical approach. The core of the photocatalytic oxidation technology is a photocatalyst, so it is important to find a photocatalyst which has good photocatalytic activity and stable performance and is more suitable for practical application.
Zinc oxide has received extensive attention and acceptance as an important photocatalyst, and it is well known that the microscopic morphology of zinc oxide has a large influence on its photocatalytic activity. Wherein, the photocatalysis characteristic of the zinc oxide one-dimensional nano structure is more prominent. For example: the research shows that the one-dimensional nanorods can provide a convenient transportation channel for the photo-generated carriers, accelerate the migration rate of the photo-generated carriers and improve the photo-catalytic efficiency.
However, there are a number of drawbacks associated with the current methods of preparing one-dimensional zinc oxide nanorods. First, in the previous studies, zinc oxide nanorods or zinc oxide nanoarrays need to be grown on zinc sheet substrates, and the preparation process is also complicated. In addition, the morphology of the obtained zinc oxide nanorods was in a non-uniform state even without the aid of a zinc sheet substrate.
Disclosure of Invention
In view of the above, the present invention aims to provide a method for preparing hexagonal-prism-shaped zinc oxide, which can prepare hexagonal-prism-shaped zinc oxide with uniform morphology without using a zinc substrate.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a method for preparing hexagonal prism-shaped zinc oxide, which comprises the following steps:
mixing a magnesium ion-containing solution and a sodium hydroxide solution, and performing substitution reaction to obtain a magnesium hydroxide-containing suspension;
and mixing the magnesium hydroxide-containing suspension with zinc salt, and performing hydrothermal reaction to obtain hexagonal prism-shaped zinc oxide.
Preferably, the magnesium salt corresponding to magnesium ions in the magnesium ion-containing solution is magnesium sulfate.
Preferably, the molar ratio of magnesium ions in the magnesium ion-containing solution to sodium hydroxide in the sodium hydroxide solution is 1:2.
Preferably, the zinc salt comprises zinc chloride.
Preferably, the molar ratio of magnesium ions to zinc salts in the magnesium ion-containing solution is 1:1.
Preferably, the temperature of the hydrothermal reaction is 100-120 ℃.
Preferably, the hydrothermal reaction time is 6-12 hours.
Preferably, after the hydrothermal reaction is completed, the method further comprises: and washing and drying the reactant obtained by the hydrothermal reaction in sequence.
Preferably, the washing comprises alcohol washing and water washing which are sequentially carried out; the times of the alcohol washing and the water washing are 3 times.
Preferably, the drying temperature is 60 ℃ and the drying time is 12 hours.
The invention provides a method for preparing hexagonal prism-shaped zinc oxide, which comprises the following steps: mixing a magnesium ion-containing solution and a sodium hydroxide solution, and performing substitution reaction to obtain a magnesium hydroxide-containing suspension; and mixing the magnesium hydroxide-containing suspension with zinc salt, and performing hydrothermal reaction to obtain hexagonal prism-shaped zinc oxide. The invention reacts magnesium ions with sodium hydroxide to generate hexagonal flake Mg (OH) through substitution reaction 2 Crystals, then subjecting the obtained hexagonal columnar crystals Mg (OH) 2 With zinc salt, because the stability constant of zinc hydroxide is higher than that of magnesium hydroxide, zn 2+ Will take Mg (OH) 2 Hydroxyl ions in the crystal grow along a (0001) crystal face by taking the hydroxyl ions as a template to generate Zn (OH) 2 The hexagonal prism-shaped zinc oxide with uniform morphology is generated through hydrothermal reaction.
The hexagonal prism-shaped zinc oxide with uniform appearance can be prepared without a zinc substrate, the method is simple, green and environment-friendly, no other surfactant is needed, and the method is suitable for large-scale preparation.
In addition, the hexagonal prism-shaped zinc oxide obtained by the method has stronger degradation capability on the diazo dye congo red.
Drawings
FIG. 1 is a schematic diagram of the preparation of hexagonal-prism-shaped zinc oxide according to the present invention;
FIG. 2 is a scanning electron microscope image of hexagonal-prism-shaped zinc oxide prepared in example 1 at different magnifications;
FIG. 3 is an XRD pattern of hexagonal-prism-shaped zinc oxide prepared in example 1;
fig. 4 is a graph showing the CR efficiency of photocatalytic degradation of hexagonal-prism-shaped zinc oxide prepared in example 1.
Detailed Description
The invention provides a method for preparing hexagonal prism-shaped zinc oxide, which comprises the following steps:
mixing a magnesium ion-containing solution and a sodium hydroxide solution, and performing substitution reaction to obtain a magnesium hydroxide-containing suspension;
and mixing the magnesium hydroxide-containing suspension with zinc salt, and performing hydrothermal reaction to obtain hexagonal prism-shaped zinc oxide.
The present invention is not limited to the specific source of the raw materials used, and may be commercially available products known to those skilled in the art, unless otherwise specified.
The invention mixes the magnesium ion-containing solution and the sodium hydroxide solution to carry out substitution reaction to obtain the magnesium hydroxide-containing suspension.
In the invention, the magnesium salt corresponding to magnesium ions in the magnesium ion-containing solution is preferably magnesium sulfate; the molar ratio of magnesium ions in the magnesium ion-containing solution to sodium hydroxide in the sodium hydroxide solution is preferably 1:2.
In the present invention, the preparation method of the magnesium ion-containing solution preferably comprises dissolving the corresponding magnesium salt in the magnesium ion-containing solution in water; the ratio of the molar amount of magnesium salt to the volume of water is preferably 1mol:15mL; the preparation method of the sodium hydroxide solution is preferably to dissolve sodium hydroxide in water; the molar amount of sodium hydroxide to volume of water ratio is preferably 2mol:15mL.
In the present invention, the mixing process of the magnesium ion-containing solution and the sodium hydroxide solution is preferably to add the magnesium ion-containing solution dropwise to the sodium hydroxide solution; the substitution reaction is preferably carried out under stirring; the stirring time is preferably 30min; the stirring process is not particularly limited, and the stirring process well known in the art is adopted to fully react the materials.
After the magnesium hydroxide-containing suspension is obtained, the magnesium hydroxide-containing suspension and zinc salt are mixed and subjected to hydrothermal reaction to obtain hexagonal prism zinc oxide.
In the present invention, the zinc salt preferably comprises zinc chloride; the molar ratio of magnesium ions to zinc salt in the magnesium ion-containing solution is preferably 1:1.
In the present invention, the mixing process of the magnesium hydroxide-containing suspension and the zinc salt is preferably to add the zinc salt to the magnesium hydroxide-containing suspension and stir the mixture; the stirring time is preferably 10min. The stirring process is not particularly limited, and the materials are uniformly mixed by adopting a stirring process well known in the art.
In the present invention, the temperature of the hydrothermal reaction is preferably 100 to 120 ℃, more preferably 110 to 120 ℃; the time of the hydrothermal reaction is preferably 6 to 12 hours, more preferably 8 to 12 hours; the equipment for the hydrothermal reaction is preferably a polytetrafluoroethylene autoclave.
In the present invention, after the completion of the hydrothermal reaction, it is preferable to further include: and washing and drying the reactant obtained by the hydrothermal reaction in sequence.
In the present invention, the washing liquid used for the washing preferably includes alcohol washing and water washing which are sequentially performed; the times of the alcohol washing and the water washing are preferably 3 times; the drying temperature is preferably 60 ℃ and the drying time is preferably 12 hours; the drying mode is preferably drying; the drying time is not particularly limited, and may be determined according to actual conditions.
FIG. 1 is a schematic diagram of the preparation of hexagonal-prism-shaped zinc oxide according to the present invention. As shown in figure 1, magnesium sulfate and sodium hydroxide react to generate regular hexagonal platy magnesium hydroxide crystals, and then hydrothermal reaction is carried out on aqueous magnesium hydroxide and zinc ions for 12 hours at 120 ℃ to generate hexagonal prism zinc oxide.
The technical solutions of the present invention will be clearly and completely described in the following in connection with the embodiments of the present invention.
Example 1
2mmol of anhydrous magnesium sulfate is dissolved in 30mL of deionized water to obtain a magnesium ion-containing solution; dissolving 4mmol of sodium hydroxide in 30mL of deionized water to obtain sodium hydroxide solution; under the action of magnetic stirring, dropwise adding a magnesium ion-containing solution into a sodium hydroxide solution to form a uniform magnesium hydroxide-containing suspension, continuously stirring for 30min, then weighing 2mmol of zinc chloride, adding into the magnesium hydroxide-containing suspension, stirring for 10min, transferring into a polytetrafluoroethylene high-pressure reaction kettle, performing hydrothermal reaction at 120 ℃ for 12h, respectively washing the obtained product with absolute ethyl alcohol and deionized water for three times, and drying at 60 ℃ for 12h to obtain hexagonal prism-shaped zinc oxide which is white powder and is marked as h-ZnO-NR.
Performance testing
(1) The hexagonal prism-shaped zinc oxide prepared in example 1 was subjected to scanning electron microscope test, and the result is shown in fig. 2, wherein a is the morphology structure of the hexagonal prism-shaped zinc oxide at low magnification, and b is the morphology structure of the hexagonal prism-shaped zinc oxide at high magnification.
As can be seen from FIG. 2, the zinc oxide prepared by the method has uniform morphology and no agglomeration phenomenon, and the cross section of the zinc oxide can be clearly observed to be hexagonal under high multiplying power.
(2) The hexagonal prism-shaped zinc oxide prepared in example 1 was subjected to an X-ray diffraction test, and the result is shown in fig. 3.
As can be seen from fig. 3, the characteristic diffraction peaks appearing in the XRD spectrum of the zinc oxide prepared according to the present invention are consistent with the corresponding standard card PDF # 65-3411.
(3) 0.05g of the h-ZnO-NR photocatalyst prepared in example 1 was weighed, added into 50mL of Congo red solution (initial concentration: 30 mg/L), and transferred into a photocatalytic reactor after ultrasonic dispersion, the system was stirred in the dark for 30min until adsorption-desorption equilibrium before illumination, and photocatalytic degradation was performed under simulated sun illumination conditions (light source: PLS-FX300DUV, configuration of AM=1.5 filter), and experimental results are shown in FIG. 4.
As can be seen from FIG. 4, the degradation efficiency of h-ZnO-NR on Congo red after 60min of illumination is 89.74%.
Although the foregoing embodiments have been described in some, but not all, embodiments of the invention, according to which one can obtain other embodiments without inventiveness, these embodiments are all within the scope of the invention.
Claims (8)
1. A method for preparing hexagonal-prism-shaped zinc oxide, comprising the steps of:
dropwise adding the magnesium ion-containing solution into a sodium hydroxide solution to obtain a magnesium hydroxide-containing suspension;
the molar ratio of magnesium ions in the magnesium ion-containing solution to sodium hydroxide in the sodium hydroxide solution is 1:2;
mixing the magnesium hydroxide-containing suspension with zinc salt, and performing hydrothermal reaction to obtain hexagonal prism-shaped zinc oxide;
the molar ratio of magnesium ions to zinc salts in the magnesium ion-containing solution is 1:1.
2. The method of claim 1, wherein the magnesium salt corresponding to magnesium ions in the magnesium ion-containing solution is magnesium sulfate.
3. The method according to claim 1, characterized in that the zinc salt comprises zinc chloride.
4. The method of claim 1, wherein the hydrothermal reaction is at a temperature of 100-120 ℃.
5. The method of claim 1, wherein the hydrothermal reaction time is 6-12 hours.
6. The method of claim 1, further comprising, after completion of the hydrothermal reaction: and washing and drying the reactant obtained by the hydrothermal reaction in sequence.
7. The method according to claim 6, wherein the washing comprises an alcohol washing and a water washing performed sequentially; the times of the alcohol washing and the water washing are 3 times.
8. The method of claim 6, wherein the drying is at a temperature of 60 ℃ for a period of 12 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210710924.5A CN115072765B (en) | 2022-06-22 | 2022-06-22 | Method for preparing hexagonal prism-shaped zinc oxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210710924.5A CN115072765B (en) | 2022-06-22 | 2022-06-22 | Method for preparing hexagonal prism-shaped zinc oxide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN115072765A CN115072765A (en) | 2022-09-20 |
| CN115072765B true CN115072765B (en) | 2023-06-23 |
Family
ID=83253614
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210710924.5A Active CN115072765B (en) | 2022-06-22 | 2022-06-22 | Method for preparing hexagonal prism-shaped zinc oxide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115072765B (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102199003A (en) * | 2010-03-23 | 2011-09-28 | 中国科学院合肥物质科学研究院 | Porous membrane with two-dimensional ordered arrangement, and preparation method thereof |
| CN103204538A (en) * | 2013-04-26 | 2013-07-17 | 通化师范学院 | Preparation method of porous ZnO and ZnO/Ag nanometer free-standing film |
| KR20180099517A (en) * | 2017-02-28 | 2018-09-05 | 전남대학교산학협력단 | Method for manufacturing magnesium hydroxide |
| WO2018159986A1 (en) * | 2017-02-28 | 2018-09-07 | 전남대학교산학협력단 | Method for preparing high-purity magnesium hydroxide |
| CN109399692A (en) * | 2018-11-23 | 2019-03-01 | 河南师范大学 | A kind of preparation method of self assembly hexagonal prisms zinc oxide |
| KR20220003406A (en) * | 2020-07-01 | 2022-01-10 | 주식회사 엘지화학 | Metal oxide nano particles, electron transport layers, quantum dot light-emitting devices comprising the same and fabricating methods thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP6456365B2 (en) * | 2014-05-01 | 2019-01-23 | 日本碍子株式会社 | Method for producing hexagonal plate-like zinc oxide particles |
-
2022
- 2022-06-22 CN CN202210710924.5A patent/CN115072765B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102199003A (en) * | 2010-03-23 | 2011-09-28 | 中国科学院合肥物质科学研究院 | Porous membrane with two-dimensional ordered arrangement, and preparation method thereof |
| CN103204538A (en) * | 2013-04-26 | 2013-07-17 | 通化师范学院 | Preparation method of porous ZnO and ZnO/Ag nanometer free-standing film |
| KR20180099517A (en) * | 2017-02-28 | 2018-09-05 | 전남대학교산학협력단 | Method for manufacturing magnesium hydroxide |
| WO2018159986A1 (en) * | 2017-02-28 | 2018-09-07 | 전남대학교산학협력단 | Method for preparing high-purity magnesium hydroxide |
| CN109399692A (en) * | 2018-11-23 | 2019-03-01 | 河南师范大学 | A kind of preparation method of self assembly hexagonal prisms zinc oxide |
| KR20220003406A (en) * | 2020-07-01 | 2022-01-10 | 주식회사 엘지화학 | Metal oxide nano particles, electron transport layers, quantum dot light-emitting devices comprising the same and fabricating methods thereof |
Non-Patent Citations (5)
| Title |
|---|
| Synthesis of nano-sized ZnO structure in ionic liquid;Chen quanshui 等;《2008 2nd IEEE International Nanoelectronics Conference》;第297-299页 * |
| ZnO晶体形貌调控、离子掺杂及其生长动力学;刘清波;《中国博士学位论文全文数据库》(第11期);全文 * |
| 氢氧化镁在强碱水热体系中的晶体生长研究;赵华;闪俊杰;刘润静;刘忻瑜;胡永琪;杜振雷;;无机盐工业(10);全文 * |
| 离子液体中片状纳米ZnO的制备、表征及其光催化性能;周咏梅 等;《大连工业大学学报》;第27卷(第1期);第70-72页 * |
| 纳米氢氧化镁的合成与结晶机理分析;印万忠,南黎,韩跃新,袁致涛,王泽红;金属矿山(03);全文 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN115072765A (en) | 2022-09-20 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102631939B (en) | Graphene/silver phosphate composite visible light photocatalyst and preparation method thereof | |
| CN111420664B (en) | Preparation method of flaky cuprous oxide/cobaltous oxide nanocomposite and application of flaky cuprous oxide/cobaltous oxide nanocomposite in catalyzing ammonia borane hydrolysis hydrogen production | |
| CN112536046B (en) | Preparation method of flaky indium zinc sulfide photocatalyst with efficient reduction activity | |
| CN110512228B (en) | Preparation method of nickel phosphide/nickel foam electrochemical functional hydrogen evolution material | |
| CN105645459B (en) | A kind of surface modification sea urchin shape ZnO/TiO2Composite and preparation method thereof | |
| TWI776041B (en) | Method for reducing carbon dioxide to manufacture carbon compound | |
| CN108311162A (en) | A kind of preparation method and applications of ZnO/BiOI heterojunction photocatalysts | |
| CN107185547A (en) | A kind of C/Fe FeVO4Composite photo-catalyst and its preparation method and application | |
| CN110589886A (en) | Preparation method of bismuth oxycarbonate | |
| CN109201083A (en) | A kind of nano flower-like vanadium disulfide/difunctional composite electrocatalyst of hydroxyl vanadium oxide and preparation method thereof | |
| CN108686658A (en) | A kind of C-QDs-Fe2O3/TiO2Composite photo-catalyst and preparation method thereof | |
| CN103754935B (en) | Method for synthesizing lead molybdate tower crystal at room temperature | |
| CN105771958B (en) | A kind of Bi4V2O11The preparation method of nano particle | |
| CN115072765B (en) | Method for preparing hexagonal prism-shaped zinc oxide | |
| CN104815665A (en) | Preparation method of Fe<3+>-doped nano ZnO photo-catalyst | |
| CN104857975A (en) | Preparation method and application of CdIn2S4-graphene composite photocatalyst | |
| CN106384832A (en) | ZnO-CuO/rGO (reduced graphene oxide) composite material with efficient electrocatalytic oxygen reduction performance | |
| CN102408132A (en) | Method for preparing nanometer lanthanum ferrite powder by using microwave process | |
| CN103785425A (en) | Preparation method and application of flower-like Bi2O(OH)2SO4 photocatalyst | |
| CN103272624B (en) | A kind of preparation method of bismuth phosphate photocatalyst | |
| CN117582977A (en) | LCQDs/Bi for degrading tetracycline 2 MoO 6 Preparation method and application of spherical flower-shaped composite photocatalyst | |
| CN109569624B (en) | Method for growing Co-doped ZnO nano-array catalyst for water electrolysis and oxygen evolution reaction and application | |
| CN115518649B (en) | (CoCuZnMnMg) 3 O 4 Preparation method of high-entropy oxide | |
| CN111013565A (en) | Ytterbium and erbium doped titanium dioxide/attapulgite nano composite material and preparation method and application thereof | |
| CN110467221A (en) | A kind of NaV6O15The preparation method of film and NaV obtained6O15Film |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |