Method for preparing nickel-cobalt-manganese hydroxide

09815709 · 2017-11-14

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Abstract

A method for preparing nickel-cobalt-manganese hydroxide. The method comprises the following steps: (1) dissolving microcrystalline cellulose into water to obtain a suspension; and adding a nickel source, a cobalt source, and a manganese source into the suspension to obtain a solution containing nickel, cobalt, and manganese; (2) adding hexamethylenetetramine into the solution containing nickel, cobalt, and manganese, heating the reaction solution to 80-90° C., and reacting for 5-10 min, then heating with a microwave hydrothermal synthesis instrument at a frequency of 2450 MHz for 10-60 min; and (3) filtering the reaction solution obtained in step (2), and taking the filter residue, washing the filter residue with pure water and ethanol respectively, then drying, crushing, and screening the filter residue to obtain nickel-cobalt-manganese hydroxide. Nickel-cobalt-manganese hydroxide prepared from the abovementioned method has a uniform particle size and consistent morphology and structure; thus solving the problems of the uncontrollable appearance and structure and the inconsistent performances of the product caused by the vigorous reaction in the existing method for preparing nickel-cobalt-manganese hydroxide.

Claims

1. A method for preparing nickel-cobalt-manganese hydroxide, comprising the following steps: (1) dissolving microcrystalline cellulose into water, and stirring to homogeneity to obtain a suspension; adding a nickel source, a cobalt source, and a manganese source into the suspension, wherein the mass ratio among the nickel source, the cobalt source, and the manganese source is (1-3):1:(1-1.5), and the ratio between the total mass of the nickel source, the cobalt source, and the manganese source and the mass of the microcrystalline cellulose is (1-3):1, and stirring to homogeneity to obtain a solution containing nickel, cobalt, and manganese; (2) adding hexamethylenetetramine into the solution containing nickel, cobalt, and manganese, making the ratio between the total mass of the nickel source, the cobalt source, and the manganese source and the mass of the hexamethylenetetramine being 1:(1-5), and stirring to homogeneity to obtain a reaction solution; heating the reaction solution to 80-90° C., and then reacting the reaction solution that has been heated to 80-90 ° C. for 5-10 min, and then heating the reaction solution that has been reacted for 5-10 min with a microwave hydrothermal synthesis instrument at a frequency of 2450 MHz for 10-60 min; (3) filtering the reaction solution obtained in step (2) after the heating the reaction solution with the microwave hydrothermal synthesis instrument, and taking filter residue, washing the filter residue with pure water and ethanol respectively, then drying, crushing, and screening the filter residue, thus obtaining nickel-cobalt-manganese hydroxide.

2. The method for preparing nickel-cobalt-manganese hydroxide according to claim 1, characterized in that the nickel source is one of nickel acetate, nickel chloride or nickel sulfate.

3. The method for preparing nickel-cobalt-manganese hydroxide according to claim 1, characterized in that the cobalt source is one of cobalt acetate, cobalt chloride or cobalt sulfate.

4. The method for preparing nickel-cobalt-manganese hydroxide according to claim 1, characterized in that the manganese source is one of manganese acetate, manganese chloride or manganese sulfate.

Description

BRIEF DESCRIPTION OF THE DRAWINGS

(1) FIG. 1 shows a scanning electron micrograph of nickel-cobalt-manganese hydroxide prepared in example 1.

DETAILED DESCRIPTION

(2) The present invention is further illustrated in detail below in combination with the examples and the drawings, but the embodiments of the present invention are not limited thereto.

EXAMPLE 1

(3) A method for preparing nickel-cobalt-manganese hydroxide, comprising the following steps:

(4) (1) dissolving 2 g of microcrystalline cellulose into 80 mL of water, and stirring to homogeneity to obtain a suspension; adding 1 g of nickel acetate, 1 g of cobalt acetate, and 1 g of manganese acetate into the suspension, and stirring to homogeneity to obtain a solution containing nickel, cobalt, and manganese;

(5) (2) adding 3 g of hexamethylenetetramine into the solution containing nickel, cobalt, and manganese, and stirring to homogeneity to obtain a reaction solution; heating the reaction solution to 80° C. and reacting for 5 min, then heating with a microwave hydrothermal synthesis instrument (Type No.: XH-800S-10 from Beijing XiangHu Science and Technology Development Co., Ltd, hereinafter) at a frequency of 2450 MHz for 30 min.

(6) (3) filtering the reaction solution obtained in step (2), and taking the filter residue, washing the filter residue with pure water and ethanol respectively, then drying the filter residue at 60° C., crushing, and screening, thus obtaining nickel-cobalt-manganese hydroxide.

(7) As shown in FIG. 1, the obtained nickel-cobalt-manganese hydroxide had a uniform particle size of about 10 μm, consistent spherical morphology, and consistent structure.

(8) EXAMPLE 2

(9) A method for preparing nickel-cobalt-manganese hydroxide, comprising the following steps:

(10) (1) dissolving 4 g of microcrystalline cellulose into 100 mL of water, and stirring to homogeneity to obtain a suspension; adding 2 g of nickel chloride, 2 g of cobalt chloride, and 2 g of manganese chloride into the suspension, and stirring to homogeneity to obtain a solution containing nickel, cobalt, and manganese;

(11) (2) adding 6 g of hexamethylenetetramine into the solution containing nickel, cobalt, and manganese, and stirring to homogeneity to obtain a reaction solution; heating the reaction solution to 90° C. and reacting for 10 min, then heating with a microwave hydrothermal synthesis instrument at a frequency of 2450 MHz for 60 min.

(12) (3) filtering the reaction solution obtained in step (2), and taking the filter residue, washing the filter residue with pure water and ethanol respectively, then drying the filter residue at 60° C., crushing, and screening, thus obtaining nickel-cobalt-manganese hydroxide.

(13) Nickel-cobalt-manganese hydroxide prepared in this example had a similar particle size and morphology as those in example 1, with a uniform particle size of about 10 μm, consistent spherical morphology, and consistent structure.

(14) The abovementioned examples are the preferred embodiments of the present invention, but the embodiments of the present invention are not limited thereto. Any other changes, modifications, alternatives, combinations, and simplifications, all of which shall be the equivalent replacements, without departing from the spirit principle of the present invention, should be included in the scope of protection of the present invention.