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

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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 difficu

Method used

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

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[0034] Example one

[0035] a. Preparation of chitosan template: dissolve corn starch (purchased from Tianjin Ruijinte Chemical Co., Ltd.) in DMSO, heat and dissolve at 95° C. for 0.5 h to prepare a 0.25 wt.% solution. After cooling to room temperature, put it in a refrigerator at 4°C and freeze, then centrifuge at 4000rpm for 15min. Repeated freezing and centrifugation for 3 times to remove large gel particles and used as a stock solution for practical use;

[0036] b. Preparation of copper source: Weigh copper chloride to prepare a 0.5M solution for later use;

[0037] c. Preparation of sulfur source: Weigh sodium thiosulfate to prepare a 0.5M solution for later use;

[0038] Take 18.4mL, 0.25wt% corn starch solution, stir in 70℃ oil bath, then add 0.8mL, 0.5M copper chloride solution to corn starch solution and stir for 30min to obtain a light blue transparent solution , The transmission electron microscope photo of the transparent solution is as figure 1 As shown, the measured di...

Example Embodiment

[0039] Example 2

[0040] a. Preparation of chitosan template: dissolve chitosan (purchased from Tianjin Ruijinte Chemical Co., Ltd.) in deionized water, heat and dissolve at 25°C for 1 hour, prepare a 0.1 wt.% solution, and cool to room temperature Then put it in a refrigerator at 8°C, and then centrifuge at 3500rpm for 20 minutes. After repeated freezing and centrifugation twice to remove large gel particles, it can be used as a stock solution;

[0041] b. Preparation of copper source: Weigh copper nitrate to prepare a 0.01M solution for later use;

[0042] c. Preparation of sulfur source: Weigh sodium sulfide to prepare a 0.01M solution for later use;

[0043] Take 18.4mL, 0.1wt% chitosan solution, stir in 30℃ oil bath, then add 0.0368mL, 0.01M copper chloride solution to the chitosan solution and stir for 24min to obtain a light blue Transparent solution, then 0.0736mL, 0.01M sodium thiosulfate was quickly added to the reaction, heated and stirred at 30°C for 24h to obtain a blac...

Example Embodiment

[0044] Example 3

[0045] a. Preparation of corn starch template: Dissolve corn starch (Tianjin Ruijinte Chemical Co., Ltd.) in acetone, heat and dissolve at 100° C. for 0.5 h to prepare a 0.5 wt.% solution. After cooling to room temperature, put it in the refrigerator and freeze it, then centrifuge at 8000rpm for 3min. Repeated freezing and centrifugation for 5 times to remove large gel particles and use it as a stock solution;

[0046] b. Preparation of copper source: Weigh copper acetate to prepare a 1M solution for use;

[0047] c. Preparation of sulfur source: Weigh potassium sulfide to prepare a 1M solution for later use;

[0048] Take 18.4 mL of corn starch solution and stir in an oil bath at 90°C. Then, add 6.44 mL of 1M copper chloride solution to the corn starch solution and stir for 30 minutes to obtain a light blue transparent solution. Then add 9.568 mL, 0.1M sodium thiosulfate was quickly added to the reaction, heated and stirred at 90°C for 2h to obtain a black suspens...

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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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