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Preparation method of submicron CuS (copper sulphide) classification ball

A sub-micron, copper sulfide technology, applied in copper sulfide and other directions, can solve the problems that the graded spherical structure of copper sulfide is difficult to achieve, environmental protection and physical health are unfavorable, and the synthesis conditions are harsh, and it is convenient for large-scale industrial production. Inexpensive equipment and simple operation

Inactive Publication Date: 2011-05-04
GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The preparation methods of copper sulfide with different morphological structures above have the following disadvantages: (1) the organic solvent used has greater toxicity, which is unfavorable to environmental protection and health; (2) the synthesis conditions are harsh; (3) the operation is complicated ; (4) hierarchical spherical structure copper sulfide is difficult to achieve
In short, it is difficult for the above methods to simultaneously realize the controllable shape and size and the environment-friendly preparation of copper sulfide. Therefore, it is very important to invent a method for preparing copper sulfide nanostructures with a relatively simple process, environmental friendliness, and better hierarchical spherical structure.

Method used

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  • Preparation method of submicron CuS (copper sulphide) classification ball

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Embodiment 1

[0035] a. Preparation of chitosan template: cornstarch (purchased from Tianjin Ruijinte Chemical Co., Ltd.) was dissolved in DMSO, heated and dissolved at 95° C. for 0.5 h, and prepared into a 0.25 wt.% solution. After cooling to room temperature, place it in a refrigerator at 4°C to freeze, then centrifuge at 4000rpm for 15 minutes, repeat this process for 3 times to remove large gel particles, and then use it as a stock solution;

[0036] b. Preparation of copper source: take cupric chloride and be mixed with 0.5M solution for subsequent use;

[0037] c. Preparation of sulfur source: take sodium thiosulfate and prepare a 0.5M solution for subsequent use;

[0038]Take 18.4mL of 0.25wt% cornstarch solution and stir in an oil bath at 70°C, then add 0.8mL of 0.5M copper chloride solution into the cornstarch solution and stir for 30min to obtain a light blue transparent solution , the transmission electron micrograph of the transparent solution is shown as figure 1 As shown, th...

Embodiment 2

[0040] a. Preparation of chitosan template: Dissolve chitosan (purchased in Tianjin Ruijinte Chemical Co., Ltd.) in deionized water, heat and dissolve at 25°C for 1h, prepare a 0.1wt.% solution, and cool to room temperature Then put it in the refrigerator at 8°C to freeze, then centrifuge at 3500rpm for 20min, repeat the process of freezing and centrifuging twice to remove large gel particles, and then use it as a stock solution;

[0041] b. Preparation of copper source: take copper nitrate and prepare a 0.01M solution for subsequent use;

[0042] c. Preparation of sulfur source: take sodium sulfide and prepare a 0.01M solution for subsequent use;

[0043] Get 18.4mL, 0.1wt% chitosan solution, stir in 30 ℃ oil bath, then, add 0.0368mL, 0.01M cupric chloride solution into chitosan solution and stir for 24min, obtain a light blue Transparent solution, then quickly add 0.0736mL, 0.01M sodium thiosulfate to the reaction, heat and stir at 30°C for 24h to obtain a black suspension,...

Embodiment 3

[0045] a. Preparation of cornstarch template: cornstarch (Tianjin Ruijinte Chemicals Co., Ltd.) was dissolved in acetone, heated and dissolved at 100°C for 0.5h, and prepared into a 0.5wt.% solution. After cooling to room temperature, put it in the refrigerator to freeze, and then centrifuge at 8000rpm for 3 minutes, repeat this way for 5 times to remove large gel particles and use it as a stock solution;

[0046] b. Preparation of copper source: take copper acetate and prepare a 1M solution for subsequent use;

[0047] c. Preparation of sulfur source: take potassium sulfide and prepare a 1M solution for subsequent use;

[0048] Take 18.4mL of cornstarch solution and stir in an oil bath at 90°C, then add 6.44mL of 1M copper chloride solution into the cornstarch solution and stir for 30min to obtain a light blue transparent solution, then add 9.568mL, Add 0.1M sodium thiosulfate to the reaction quickly, heat and stir at 90°C for 2 hours to obtain a black suspension, then trans...

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Abstract

The invention discloses a preparation method of submicron CuS (copper sulphide) classification balls. The method comprises the following steps: adding polymer into a good solvent to dissolve and remove big gel particles; adding copper source solution to the good solvent and stirring; adding sulfur source solution and then stirring; reacting the reaction liquid under 100-1,000 KPa at 100-200 DEG C; naturally cooling to the room temperature to obtain black precipitate; and washing and drying the precipitate to obtain the classification balls. The classification balls has the advantages of cheap and readily available templates, environmental friendliness, safety without toxicity, renewability and high water solubility, the contents of raw materials are abundant in nature and the operation of the reaction system is simple; the size and structure of the prepared classification ball are adjustable: the diameter can be controlled by adjusting the molar weight of the added precursor, the template concentration, the reaction temperature and time and the like; the operation is simple; and the prepared classification balls have wide application value in the fields of catalyst, catalyst carrier, optical equipment, sensor, lithium-ion rechargeable battery cathode material, superconductor and the like.

Description

technical field [0001] The invention relates to the field of inorganic nanometer materials and functional materials, in particular to a method for preparing submicron CuS graded spheres using polymers as templates. Background technique [0002] Copper sulfide (CuS) nanoparticles are a P-type semiconductor, which has the following advantages: (1) It has good optical properties such as visible light absorption, infrared transmission, photoluminescence, and large nonlinear polarizability. It has potential application value in the fields of photocontrol devices, photocatalysts and photoelectrodes; (2) it has the characteristics of high conductivity and high energy capacitance, so it is an excellent cathode material in lithium-ion batteries; (3) when the temperature is equal to 1.6K, It exhibits excellent superconducting properties, so it is also a good low-temperature superconducting material. In addition, it can also be used as a high-temperature fast ion conductor material, a...

Claims

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Application Information

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IPC IPC(8): C01G3/12
Inventor 胡继文李银辉肖定书胡美龙
Owner GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI
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