CN102190334A - Method for preparing trihydroxy cobalt hydroxide - Google Patents
Method for preparing trihydroxy cobalt hydroxide Download PDFInfo
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- CN102190334A CN102190334A CN 201010117854 CN201010117854A CN102190334A CN 102190334 A CN102190334 A CN 102190334A CN 201010117854 CN201010117854 CN 201010117854 CN 201010117854 A CN201010117854 A CN 201010117854A CN 102190334 A CN102190334 A CN 102190334A
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Abstract
The invention relates to a method for preparing trihydroxy cobalt hydroxide, which comprises the following steps of: adding an appropriate amount of cobalt chloride and hexadecyl trimethyl ammonium chloride into mixed liquor of N,N-dimethylformamide and deionized water, and slightly stirring to form red uniform solution; adding 30 weight percent of hydrogen peroxide, fully mixing, screwing a reaction kettle, putting into a drying box, and standing at the temperature of 150 DEG C; and performing centrifugal separation on a product, and washing for multiple times to obtain the product. Compared with the prior art, the method has the advantages that: a new type of trihydroxy cobalt hydroxide is synthesized by a hydrothermal method, is well crystallized, and has controllable size and structure, high purity and definite components; the preparation method is simple and practicable, and high in operability and repeatability; and the powdered product has stable performance, can be stored in air at room temperature for a long time, and can be widely used for the fields of energy batteries, catalysis, electrochemistry, gas sensors, magnetics and the like.
Description
Technical field
The present invention relates to a kind of method for preparing inorganic materials, especially relate to a kind of method for preparing the trihydroxy-cobaltous hydroxide.
Background technology
Cobaltous hydroxide is a kind of functional materials that has extensive use, and the additive that is commonly used for the Ni/MH cell positive material is to improve the electric capacity and specific conductivity " the Synthesis of CoOOH nanorods andapplication as coating materials of nickel hydroxide for high temper of β-NiOOH battery
The preparation of cobaltous hydroxide at present is the focus of research.Some synthetic methods such as liquid-phase precipitation " Synthesis ofthe CoOOH fine nanoflake film with the high rate capacitance property " [Hosono E, Fujihara S, Honma I, IchiharaM and Zhou H S J.Power Sources, 158,779-783 (2006)], presoma transforms " Microwave-assisted synthesis of β-C (OH)
2And Co3O4nanosheets via a layered precursor conversion method " [Liang Z; Zhu Y; Cheng G andHuang Y.Can.J.Chem.84; 1050-1053 (2006)] and electrochemical deposition method " Directlow-temperature deposition of crystallized CoOOH films by potentiostatic electrolysis " [Pauporte T; Mendoza L; Cassir M, Bernard M C and Chivote J.J.electrochem.Soc.152, C49-C53 (2005)] etc. be used for carrying out the preparation of cobaltous hydroxide product, but, cobaltous hydroxide kind related in the current various preparation research is limited, has only β-C (OH) usually
2With two kinds of CoOOH; And, because it is not the crystal structure properties of cobaltous hydroxide own, high by the Adjustable structure control of above-mentioned approach institute synthetic product.This can limit the cobaltous hydroxide material greatly in the research of each related fields and the optimization and the raising of application performance.
Therefore, explore a kind of preparation method of cobaltous hydroxide product of synthetic new kind, carry out the synthetic of trihydroxy-cobaltous hydroxide, a kind of research model of cobaltous hydroxide not only is provided in theory, and having increased the chance that obtains high-performance cobaltous hydroxide device in actual applications, this is significant for Application Areas and the application prospect of expanding cobaltous hydroxide.
Summary of the invention
Purpose of the present invention is exactly to provide in order to overcome the defective that above-mentioned prior art exists that a kind of preparation method is easy, product purity is high, the lower-cost method for preparing the trihydroxy-cobaltous hydroxide.
Purpose of the present invention can be achieved through the following technical solutions:
A kind of method for preparing the trihydroxy-cobaltous hydroxide is characterized in that, this method may further comprise the steps:
(1) with N, N-dimethylformamide and deionized water are to be added to reactor at 1: 1 by volume, obtain mixing solutions, in mixing solutions, add cobalt chloride and palmityl trimethyl ammonium chloride then, open whipping appts and make cobalt chloride and palmityl trimethyl ammonium chloride dissolving, form red homogeneous solution;
(2) hydrogen peroxide of adding 30wt% in reactor, continue to mix, obtain mixture, screw reactor then, place 150 ℃ baking oven to heat 10-20h reactor, after the product that obtains carried out centrifugation, washing 2-4 time and drying, obtain wine-colored powdery product, be product.
The volumetric molar concentration of the cobalt chloride in the described mixture is 2.0-3.0mM.
The volumetric molar concentration of the palmityl trimethyl ammonium chloride in the described mixture is 3.0-5.0mM.
The volumetric molar concentration of the hydrogen peroxide in the described mixture is 0.04-1.6M.
The heat-up time of described reactor preferred 15-20h.
A kind of method for preparing the trihydroxy-cobaltous hydroxide according to claim 1 is characterized in that, described microstructure of product is banded, and length is that 1.5～50 μ m, width are 20nm～3 μ m.
Compared with prior art, the present invention adopts the trihydroxy-cobaltous hydroxide of the synthetic new kind of hydrothermal method, crystallization is good, product purity is high, component is definite, and the preparation method is simple, workable, good reproducibility, cost are low, the powdery product stable performance, but prolonged preservation in the air under the room temperature is expected to be widely used in fields such as energy battery, catalysis, electrochemistry, gas sensor and magnetics.
Description of drawings
Fig. 1 obtains the X-ray diffracting spectrum of product for embodiment 1.
Embodiment
The present invention is described in detail below in conjunction with the drawings and specific embodiments.
Embodiment 1
In the reactor of the tetrafluoroethylene of a 100mL, take by weighing the 0.03g cobalt chloride, 0.012g palmityl trimethyl ammonium chloride (CTAC) joins 5mL N, in the mixed solution of N-dimethylformamide and 5mL water, gentle agitation forms the homogeneous solution of a redness until the cobalt chloride dissolving fully.Under agitation add 0.05mL then, content is the hydrogen peroxide of 30wt%, mixes fully, and the volumetric molar concentration of the cobalt chloride in the solution is 2.5mM, and the volumetric molar concentration of palmityl trimethyl ammonium chloride is 4.0mM, and the volumetric molar concentration of hydrogen peroxide is 0.04M.Screw reactor, with its insert in the baking oven in 150 ℃ leave standstill 15h after, product carried out centrifugation, washing 3 times and oven dry after, obtain wine-colored powdery product.This product is a taraxacum shape nano belt assembly, the about 1.5 μ m of the length of single band, the about 20nm of width.The XRD figure spectrum shows that its crystallization is good as shown in Figure 1.
In the reactor of the tetrafluoroethylene of a 100mL, take by weighing the 0.03g cobalt chloride, 0.012g palmityl trimethyl ammonium chloride (CTAC) joins 5mL N, in the mixed solution of N-dimethylformamide and 5mL water, gentle agitation forms the homogeneous solution of a redness until the cobalt chloride dissolving fully.The hydrogen peroxide that under agitation adds 1.0mL (30%) then mixes fully, and the volumetric molar concentration of the cobalt chloride in the solution is 2.5mM, and the volumetric molar concentration of palmityl trimethyl ammonium chloride is 4.0mM, and the volumetric molar concentration of hydrogen peroxide is 0.8M.Screw reactor, with its insert in the baking oven in 150 ℃ leave standstill 15h after, product carried out centrifugation, washing 2 times and oven dry after, obtain wine-colored powdery product.This product is monodispersed acicular nanometer band, the about 10 μ m of the length of single band, and the about 2 μ m of width, XRD figure spectrum corresponding among the embodiment 2 is similar with example 1.
Embodiment 3
In the reactor of the tetrafluoroethylene of a 100mL, take by weighing the 0.03g cobalt chloride, 0.012g palmityl trimethyl ammonium chloride (CTAC) joins 5mL N, in the mixed solution of N-dimethylformamide and 5mL water, gentle agitation forms the homogeneous solution of a redness until the cobalt chloride dissolving fully.The hydrogen peroxide that under agitation adds 2.0mL (30%) then mixes fully, and the volumetric molar concentration of the cobalt chloride in the solution is 2.5mM, and the volumetric molar concentration of palmityl trimethyl ammonium chloride is 4.0mM, and the volumetric molar concentration of hydrogen peroxide is 1.6M.Screw reactor, with its insert in the baking oven in 150 ℃ leave standstill 15h after, product carried out centrifugation, washing 4 times and oven dry after, obtain wine-colored powdery product.This product is monodispersed acicular nanometer band, and the about 50 μ m of the length of single band, the about 3 μ m of width, its hysteresis curve show, are higher than this nano belt of 40K and are super paramagnetic material, and XRD figure spectrum corresponding among the embodiment 3 is similar with example 1.
Embodiment 4
A kind of method for preparing the trihydroxy-cobaltous hydroxide, this method may further comprise the steps:
(1) with N, N-dimethylformamide and deionized water are to be added to reactor at 1: 1 by volume, obtain mixing solutions, in mixing solutions, add cobalt chloride and palmityl trimethyl ammonium chloride then, open whipping appts and make cobalt chloride and palmityl trimethyl ammonium chloride dissolving, form red homogeneous solution;
(2) hydrogen peroxide of adding 30wt% in reactor, continue to mix, obtain mixing solutions, the volumetric molar concentration of the cobalt chloride in the solution is 2.0mM, the volumetric molar concentration of palmityl trimethyl ammonium chloride is 3.0mM, the volumetric molar concentration of hydrogen peroxide is 0.04M, screw reactor then, place 150 ℃ baking oven to heat 10h reactor, with the product that obtains carry out centrifugation, the washing 3 times and the oven dry after, obtain wine-colored powdery product, be product trihydroxy-cobaltous hydroxide (Co (OH)
3), the microtexture of the trihydroxy-cobaltous hydroxide that obtains is for banded, and length is about 1.5 μ m, width is about 20nm.
Embodiment 5
A kind of method for preparing the trihydroxy-cobaltous hydroxide, this method may further comprise the steps:
(1) with N, N-dimethylformamide and deionized water are to be added to reactor at 1: 1 by volume, obtain mixing solutions, in mixing solutions, add cobalt chloride and palmityl trimethyl ammonium chloride then, open whipping appts and make cobalt chloride and palmityl trimethyl ammonium chloride dissolving, form red homogeneous solution;
(2) hydrogen peroxide of adding 30wt% in reactor, continue to mix, obtain mixing solutions, the volumetric molar concentration of the cobalt chloride in the mixed solution is 3.0mM, the volumetric molar concentration of palmityl trimethyl ammonium chloride is 5.0mM, the volumetric molar concentration of hydrogen peroxide is 0.1M, screw reactor then, place 150 ℃ baking oven to heat 20h reactor, with the product that obtains carry out centrifugation, the washing 3 times and the oven dry after, obtain wine-colored powdery product, be product trihydroxy-cobaltous hydroxide (Co (OH)
3), the microtexture of the trihydroxy-cobaltous hydroxide that obtains is for banded, and length is about 50 μ m, width is about 3 μ m.
Claims (6)
1. a method for preparing the trihydroxy-cobaltous hydroxide is characterized in that, this method may further comprise the steps:
(1) with N, N-dimethylformamide and deionized water are to be added to reactor at 1: 1 by volume, obtain mixing solutions, in mixing solutions, add cobalt chloride and palmityl trimethyl ammonium chloride then, open whipping appts and make cobalt chloride and palmityl trimethyl ammonium chloride dissolving, form red homogeneous solution;
(2) hydrogen peroxide of adding 30wt% in reactor, continue to mix, obtain mixture, screw reactor then, place 150 ℃ baking oven to heat 10-20h reactor, after the product that obtains carried out centrifugation, washing 2-4 time and drying, obtain wine-colored powdery product, be product.
2. a kind of method for preparing the trihydroxy-cobaltous hydroxide according to claim 1 is characterized in that the volumetric molar concentration of the cobalt chloride in the described mixture is 2.0-3.0mM.
3. a kind of method for preparing the trihydroxy-cobaltous hydroxide according to claim 1 is characterized in that the volumetric molar concentration of the palmityl trimethyl ammonium chloride in the described mixture is 3.0-5.0mM.
4. a kind of method for preparing the trihydroxy-cobaltous hydroxide according to claim 1 is characterized in that the volumetric molar concentration of the hydrogen peroxide in the described mixture is 0.04-1.6M.
5. a kind of method for preparing the trihydroxy-cobaltous hydroxide according to claim 1 is characterized in that, the heat-up time of described reactor preferred 15-20h.
6. a kind of method for preparing the trihydroxy-cobaltous hydroxide according to claim 1 is characterized in that, the microtexture of described product is banded, and length is that 1.5～50 μ m, width are 20nm～3 μ m.
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| CN106984334A (en) * | 2017-03-13 | 2017-07-28 | 同济大学 | The synthetic method of cobalt disulfide nanobelt package assembly in a kind of titanium sheet substrate |
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| CN101434418A (en) * | 2008-12-04 | 2009-05-20 | 上海大学 | Method for preparing Co3O4 nano material by hydrothermal method under magnetic field effect |
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| CN101434418A (en) * | 2008-12-04 | 2009-05-20 | 上海大学 | Method for preparing Co3O4 nano material by hydrothermal method under magnetic field effect |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106984334A (en) * | 2017-03-13 | 2017-07-28 | 同济大学 | The synthetic method of cobalt disulfide nanobelt package assembly in a kind of titanium sheet substrate |
| CN106984334B (en) * | 2017-03-13 | 2019-12-03 | 同济大学 | The synthetic method of cobalt disulfide nanobelt package assembly in a kind of titanium sheet substrate |
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