CN107792888A - A kind of high-specific surface area ZnCo2O4Preparation method - Google Patents
A kind of high-specific surface area ZnCo2O4Preparation method Download PDFInfo
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- CN107792888A CN107792888A CN201710999420.9A CN201710999420A CN107792888A CN 107792888 A CN107792888 A CN 107792888A CN 201710999420 A CN201710999420 A CN 201710999420A CN 107792888 A CN107792888 A CN 107792888A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/40—Cobaltates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/30—Three-dimensional structures
- C01P2002/32—Three-dimensional structures spinel-type (AB2O4)
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
Abstract
The present invention relates to ZnCo2O4Preparation method, more particularly to a kind of high-specific surface area ZnCo2O4Preparation method, comprise the following steps：After zinc nitrate and cobalt nitrate are dissolved in into ethylene glycol, mixed liquor A is obtained, silica colloid solution is then added into mixed liquor A, obtain reaction solution B；Heating response liquid B after reaction terminates, obtains product C until generation combustion reaction；Washing, desciccate C, obtain high-specific surface area ZnCo2O4.ZnCo prepared by the present invention2O4Specific surface area is high, and preparation technology is simple, and reaction condition is relatively mild, easily operated, and equipment investment is few, with short production cycle, easy mass production.
Description
Technical field
The present invention relates to ZnCo2O4Preparation method, more particularly to a kind of high-specific surface area ZnCo2O4Preparation method.
Background technology
Spinel type compound is as a kind of new semiconducting compound, because with Stability Analysis of Structures, forbidden band is narrower, energy
Responding to visible light, photoelectrochemical behaviour are stable and the features such as repeatable utilization rate is high and as the focus of people's research.Wherein
ZnCo2O4Not only possess the distinctive property of spinel structure, its excellent electrochemical properties, air-sensitive property and catalytic property etc.,
Through being widely used in the fields such as ceramic material, solid-state gas sensor, different-phase catalyst, sorbing material, ultracapacitor.Close
In ZnCo2O4The preparation method of nano particle have hydrothermal synthesis method, chemical coprecipitation, sol-gel process, self-propagating high-temperature method,
Ion-exchange etc., the ZnCo that these methods are prepared2O4Although nano particle uniform particle sizes, good dispersion degree, morphology controllable but
It is that method operating process is complicated, process conditions are harsh, the production cycle is long, yields poorly, is unfavorable for industrialized production.Specifically, such as
It is described below：
《Chinese Journal of Inorganic Chemistry》1st phase in 2010 discloses one《Ion-exchange synthesizes cobalt acid zinc nano-hollow material
And magnetic》, by the use of cobaltosic oxide nano isometric particle as presoma in paper, under the hydrothermal condition of relative low temperature, pass through
Itself existing diffusion and ion exchange, are prepared for the cobalt acid zinc that particle diameter is 20nm, aperture is 8nm in reaction system
Nanometer box.The synthetic reaction first has to synthesize cobaltosic oxide nano cube, then realizes ion exchange under hydrothermal conditions, grasps
Make relatively cumbersome, yield is relatively low and is not easy industrial mass production.
《Battery》6th phase in 2013 discloses one《The preparation of porous cobalt acid Zinc material and embedding lithium performance》, in paper with
Oxalic acid is complexing agent, and presoma is made using coprecipitation, then calcines 2h in oxygen atmosphere, at 500 DEG C, prepares nanoporous
ZnCo2O4Material.Although this method can obtain porous ZnCo2O4, but technological process is cumbersome, and condition is relatively harsh.
《New Chemical Materials》2nd phase in 2013 discloses one《Hollow ZnCo2O4The synthesis of nano wire and its electrochemistry
Performance evaluation》, microemulsion method is used in paper, and using acetate as raw material, oxalic acid is precipitating reagent, and CTAB is surfactant, second
Glycol is that single solvent synthesizes presoma ZnCo first2(Co2O4)3Nano wire, then use ZnCo2(Co2O4)3Nano wire is as sacrificial
Domestic animal template synthesizes hollow ZnCo by calcining2O4Nano wire.Surfactant is used in building-up process, the synthesis path phase
To complex.
《Acta PhySico-Chimica Sinica》4th phase in 2017 discloses one《Three-dimensional meso-hole cobalt acid zinc it is cubical preparation and its it is excellent
Different storage lithium performance》, zinc acetate, cobalt acetate, sodium acid carbonate, urea are dissolved in ethanol and distilled water in paper, at 180 DEG C
Hydro-thermal reaction 24h, obtained precipitation are taken out, and after ethanol and distillation washing, then 8h are dried at 120 DEG C, obtain ZnCo2O4Before
Drive body.Presoma is placed in tube furnace, and 600 DEG C of calcining at constant temperature 2h are warming up to 2 DEG C/min speed in atmosphere, is made black
Color ZnCo2O4Powder.The synthetic method mainly includes two procedures, and calcining heat is higher, takes longer, specific surface area
(41.4m2/ g) it is relatively low.
The content of the invention
It is an object of the invention to overcome prior art ZnCo2O4A kind of the defects of specific surface area is relatively low, there is provided high-ratio surface
Product ZnCo2O4Preparation method.
The invention provides a kind of high-specific surface area ZnCo2O4Preparation method, comprise the following steps：
(1) after zinc nitrate and cobalt nitrate being dissolved in into ethylene glycol, mixed liquor A is obtained, titanium dioxide is then added into mixed liquor A
Colloidal silica solution, obtain reaction solution B；
(2) heating response liquid B is until generation combustion reaction, after reaction terminates, obtains product C；
(3) washing, desciccate C, obtain high-specific surface area ZnCo2O4。
Specifically, the mol ratio of described zinc nitrate and cobalt nitrate is 1:2.
Specifically, the volume ratio of the silica colloid solution described in described step (1) and ethylene glycol is 1:10-
50。
Specifically, the volume ratio of the silica colloid solution and ethylene glycol is 1:12.5.
Specifically, in the step (2), in heating response liquid B, heating-up temperature is 250-400 DEG C.
Specifically, in step (3), in washed product C, first with distillation water washing, then hydroxide is used at 80 DEG C
Sodium solution etch product C 24h, then with distilled water and ethanol washed product C；In desciccate C, drying temperature is 60-
110℃。
Beneficial effects of the present invention：(1) ZnCo prepared by the present invention2O4Specific surface area is high；(2) present invention in ethylene glycol not
Only play a part of solvent, fuel, and reducing agent effect is served as in combustion reaction, save raw material, reduce the production of enterprise
Cost；(3) preparation technology of the present invention is simple, and reaction condition is relatively mild, easily operated；(4) present device less investment, production
Cycle is short, easy mass production.
Embodiment
With reference to specific embodiment, the present invention is further illustrated.
Embodiment 1
In 100 milliliters of beakers, 0.595g zinc nitrates are sequentially added, 1.165g cobalt nitrates and 5.0mL ethylene glycol, stirring are filled
Dispersion liquid A is obtained after point, 0.4mL SiO are then added into dispersion liquid A2Colloidal solution, reaction solution B, ultrasonic reaction liquid B are obtained,
Ultrasonic time is 10min, then heating response liquid B to 300 DEG C, until combustion reaction occurs for reaction solution B, after question response terminates,
With distilled water washed product, then SiO is removed with sodium hydroxide solution etch product C 24h at 80 DEG C2, then successively with distillation
Water, ethanol washed product, wash respectively 3 times, finally dried at a temperature of 60 DEG C, produce ZnCo2O4Powder.With
The specific surface area analysis instrument of Quantachrome companies measures ZnCo2O4Specific surface area be 130.0m2/g。
Embodiment 2
The ZnCo of 2~embodiment of embodiment 52O4Preparation method is substantially the same manner as Example 1, and difference is shown in Table 1.
Table 1
| Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Comparative example | |
| Zinc nitrate (g) | 0.595 | 0.595 | 0.595 | 0.595 | 0.595 |
| Cobalt nitrate (g) | 1.165 | 1.165 | 1.165 | 1.165 | 1.165 |
| Silicon dioxide colloid (mL) | 0.1 | 0.2 | 0.3 | 0.5 | 0 |
| Ethylene glycol (mL) | 5 | 6 | 8 | 5 | 5 |
| Heating-up temperature (DEG C) | 250 | 300 | 350 | 400 | 300 |
| Desciccate temperature (DEG C) | 80 | 90 | 100 | 110 | 60 |
| Specific surface area (m2/g) | 64.4 | 82.5 | 120.4 | 104.6 | 28.1 |
Comparative example
The ZnCo of comparative example2O4Preparation method is substantially the same manner as Example 1, is a difference in that to remove and is walked as follows in embodiment 1
Suddenly：Then 0.4mL SiO are added into dispersion liquid A2Colloidal solution.Surveyed with the specific surface area analysis instrument of Quantachrome companies
Obtain comparative example and prepare ZnCo2O4Specific surface area be 28.1m2/g。
The above is only the section Example of the present invention, any formal limitation not done to the present invention, it is every according to
Any simple modification made according to the technical spirit of the present invention to above-described embodiment, equivalent variations and modification, belong to the present invention
In the range of technical scheme.
Claims (6)
- A kind of 1. high-specific surface area ZnCo2O4Preparation method, it is characterised in that：Comprise the following steps：(1) after zinc nitrate and cobalt nitrate being dissolved in into ethylene glycol, mixed liquor A is obtained, dioxide/silica gel is then added into mixed liquor A Liquid solution, obtain reaction solution B；(2) heating response liquid B is until generation combustion reaction, after reaction terminates, obtains product C；(3) washing, desciccate C, obtain high-specific surface area ZnCo2O4。
- 2. high-specific surface area ZnCo according to claim 12O4Preparation method, it is characterised in that：Described zinc nitrate and nitre The mol ratio of sour cobalt is 1:2.
- 3. high-specific surface area ZnCo according to claim 12O4Preparation method, it is characterised in that：In described step (1) Described silica colloid solution and the volume ratio of ethylene glycol are 1:10-50.
- 4. high-specific surface area ZnCo according to claim 12O4Preparation method, it is characterised in that：The dioxide/silica gel The volume ratio of liquid solution and ethylene glycol is 1:12.5.
- 5. high-specific surface area ZnCo according to claim 12O4Preparation method, it is characterised in that：In the step (2), During heating response liquid B, heating-up temperature is 250-400 DEG C.
- 6. according to the high-specific surface area ZnCo described in claim any one of 1-52O4Preparation method, it is characterised in that：In step (3) in, in washed product C, first with distillation water washing, sodium hydroxide solution etch product C 24h are then used at 80 DEG C, then With distilled water and ethanol washed product C, in desciccate C, drying temperature is 60-110 DEG C.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108793267A (en) * | 2018-07-19 | 2018-11-13 | 江苏理工学院 | A kind of MCo2O4The preparation method of nano wire |
| CN109133182A (en) * | 2018-09-30 | 2019-01-04 | 江苏理工学院 | A kind of preparation method of macropore Manganese Ferrite |
| CN114284082A (en) * | 2021-12-30 | 2022-04-05 | 江西科技师范大学 | Preparation method and application of high-capacitance oxygen vacancy rare earth doped cobaltosic oxide nanosheet |
| CN115007158A (en) * | 2022-05-25 | 2022-09-06 | 天津大学 | Ammonia decomposition catalyst and preparation method and application thereof |
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| CN101234751A (en) * | 2008-03-05 | 2008-08-06 | 中国科学院化学研究所 | Method for preparing nano material by flame combustion |
| CN101880052A (en) * | 2010-06-28 | 2010-11-10 | 暨南大学 | Preparation method of nanoscale lanthanum oxide |
| CN106334555A (en) * | 2016-11-15 | 2017-01-18 | 烟台大学 | High-activity and high-stability supported nanometer gold catalyst, preparation and application method |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108793267A (en) * | 2018-07-19 | 2018-11-13 | 江苏理工学院 | A kind of MCo2O4The preparation method of nano wire |
| CN109133182A (en) * | 2018-09-30 | 2019-01-04 | 江苏理工学院 | A kind of preparation method of macropore Manganese Ferrite |
| CN114284082A (en) * | 2021-12-30 | 2022-04-05 | 江西科技师范大学 | Preparation method and application of high-capacitance oxygen vacancy rare earth doped cobaltosic oxide nanosheet |
| CN114284082B (en) * | 2021-12-30 | 2023-04-28 | 江西科技师范大学 | Preparation method and application of high-capacitance oxygen vacancy rare earth doped cobaltosic oxide nano-sheet |
| CN115007158A (en) * | 2022-05-25 | 2022-09-06 | 天津大学 | Ammonia decomposition catalyst and preparation method and application thereof |
| CN115007158B (en) * | 2022-05-25 | 2024-03-22 | 天津大学 | Ammonia decomposition catalyst, preparation method and application thereof |
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Application publication date: 20180313 |