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Preparation method of sea urchin-shaped basic cobalt carbonate

A technology of cobalt carbonate and sea urchin shape, which is applied in the field of preparation of sea urchin shape basic cobalt carbonate, which can solve the problems of large structure size, difficult size control, and low aggregation density of nanowires

Active Publication Date: 2021-05-11
CHONGQING UNIV OF ARTS & SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The shortcomings of the preparation of basic cobalt carbonate are that the shape and size of the product are difficult to control, and the product purity is not high. For example, the patent CN105016319A uses cobalt nitrate and urea to dissolve in water and then hydrothermally prepares a sea urchin-like hydrated basic cobalt carbonate precursor. , and the sea urchin-like cobalt phosphide treated with the precursor of hypophosphorous acid at high temperature, but the nanowires assembled in the sea urchin-like basic cobalt carbonate have small aggregation density and poor uniformity, and the size of the structure is large and the particle size distribution uneven

Method used

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  • Preparation method of sea urchin-shaped basic cobalt carbonate
  • Preparation method of sea urchin-shaped basic cobalt carbonate

Examples

Experimental program
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Embodiment 1

[0029] A kind of preparation method of sea urchin shape cobalt basic carbonate is characterized in that, carries out as follows:

[0030] Step (1) Dissolve cobalt nitrate hexahydrate in a mixture of deionized water and ethylene glycol to form solution A. The volume ratio of deionized water and ethylene glycol is 1:1, and the amount of cobalt nitrate hexahydrate in solution A The concentration is 0.1mol / L;

[0031] Step (2) Dissolve urea in a mixed solution of ammonia water and ethylene glycol with a mass fraction of 25% to form solution B. The volume ratio of ammonia water and ethylene glycol is 1:2, and the concentration of urea in solution B is 0.3mol / L;

[0032] Step (3) Heat solution A to 75°C, according to the molar ratio of cobalt nitrate hexahydrate and urea as 1:3, add solution B dropwise to solution A at a rate of 0.2 mL / min while stirring at 160 rpm;

[0033] After the step (4) is added dropwise, a solvothermal reaction is carried out at 170°C for 2 hours;

[003...

Embodiment 2

[0038] A kind of preparation method of sea urchin shape cobalt basic carbonate is characterized in that, carries out as follows:

[0039] Step (1) Dissolve cobalt nitrate hexahydrate in a mixture of deionized water and ethylene glycol to form solution A. The volume ratio of deionized water and ethylene glycol is 1:1, and the amount of cobalt nitrate hexahydrate in solution A The concentration is 0.02mol / L;

[0040] Step (2) Dissolve urea in a mixed solution of ammonia water and ethylene glycol with a mass fraction of 25% to form solution B. The volume ratio of ammonia water and ethylene glycol is 1:1, and the concentration of urea in solution B is 0.03mol / L;

[0041] Step (3) Heat solution A to 70°C, according to the molar ratio of cobalt nitrate hexahydrate and urea as 1:3, add solution B dropwise to solution A at a rate of 0.15mL / min while stirring at 150rpm;

[0042]After the step (4) is added dropwise, a solvothermal reaction is carried out at 160°C for 5 hours;

[004...

Embodiment 3

[0046] A kind of preparation method of sea urchin shape cobalt basic carbonate is characterized in that, carries out as follows:

[0047] Step (1) Dissolve cobalt nitrate hexahydrate in a mixture of deionized water and ethylene glycol to form solution A. The volume ratio of deionized water and ethylene glycol is 1:1, and the amount of cobalt nitrate hexahydrate in solution A The concentration is 0.3mol / L;

[0048] Step (2) Dissolve urea in a mixed solution of ammonia water and ethylene glycol with a mass fraction of 25% to form solution B. The volume ratio of ammonia water and ethylene glycol is 1: 3, and the concentration of urea in solution B is 0.5mol / L;

[0049] Step (3) Heat solution A to 80°C, according to the molar ratio of cobalt nitrate hexahydrate and urea as 1:3, add solution B dropwise to solution A at a rate of 0.45mL / min while stirring at 150~180rpm ;

[0050] After the step (4) is added dropwise, a solvothermal reaction is carried out at 180°C for 1 hour;

...

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Abstract

The invention relates to a preparation method of sea urchin-shaped basic cobalt carbonate, which is characterized by comprising the following steps: dissolving cobalt nitrate hexahydrate in a mixed solution of deionized water and ethylene glycol to form a solution A, dissolving urea in a mixed solution of ammonia water with a mass fraction of 25% and ethylene glycol to form a solution B, heating the solution A to 70-80 DEG C, dropwise adding the solution B into the solution A while stirring at the speed of 150-180rpm, carrying out solvothermal reaction, conducting centrifuging after the reaction is finished to obtain a precipitate, and sequentially conducting washing and drying. The prepared sea urchin-shaped basic cobalt carbonate nano material is formed by self-assembly of a large number of one-dimensional nanorods, the nanorods radially grow from the center of a sea urchin-shaped structure, the nanorods are high in assembly density and excellent in dispersity, the nanorods are not agglomerated, the assembled sea urchin structure is regular in morphology, uniform in particle size and narrow in distribution, the particle size is about 2-2.5 micrometers, and the product has high purity and no impurity.

Description

technical field [0001] The invention relates to the technical field of nanomaterial preparation, in particular to a preparation method of sea urchin-shaped cobalt basic carbonate. Background technique [0002] Basic cobalt carbonate is a purple-red crystal or powder, mainly used to prepare various cobalt-based products such as metal cobalt powder and tricobalt tetroxide. Materials and other fields have broad application prospects and have attracted widespread attention and become a research hotspot. [0003] The shortcomings of the preparation of basic cobalt carbonate are that the shape and size of the product are difficult to control, and the product purity is not high. For example, the patent CN105016319A uses cobalt nitrate and urea to dissolve in water and then hydrothermally prepares a sea urchin-like hydrated basic cobalt carbonate precursor. , and the sea urchin-like cobalt phosphide treated with the precursor of hypophosphorous acid at high temperature, but the nan...

Claims

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Application Information

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IPC IPC(8): C01G51/06B82Y40/00
CPCC01G51/06B82Y40/00C01P2002/72C01P2002/85C01P2004/03C01P2004/61C01P2004/64C01P2004/50
Inventor 吴会杰
Owner CHONGQING UNIV OF ARTS & SCI
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