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Technology for synthesizing sulfur quantum dots through oil-water interface method

An oil-water interface method, sulfur quantum technology, applied in the preparation/purification of sulfur, nanotechnology for materials and surface science, nanotechnology, etc. and other problems, to achieve the effects of uniform particle size distribution, mild reaction conditions, and easy promotion.

Active Publication Date: 2014-02-19
MINNAN NORMAL UNIV
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

Patent name: Preparation method of high-purity nano-sulfur (patent application number: 03128015.3) discloses a method for preparing elemental sulfur by chemical vapor deposition. This method has problems such as cumbersome operation, high cost, wide particle size distribution, and difficulty in regulation. ; Patent name: Preparation of nano-sulfur particles by microemulsion method (patent application number: 201010220221.1) discloses a method for preparing elemental sulfur by microemulsion method. This method has complex reaction system, cumbersome operation, large particle size of nano-sulfur and wide distribution And other issues
The reason for this problem is that the homogeneous reaction speed is fast, and the specific surface area of ​​nano-sulfur is large, so that the particles are easily adsorbed and agglomerated, thereby forming large agglomerated particles.

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  • Technology for synthesizing sulfur quantum dots through oil-water interface method
  • Technology for synthesizing sulfur quantum dots through oil-water interface method
  • Technology for synthesizing sulfur quantum dots through oil-water interface method

Examples

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preparation example Construction

[0027] (1) Preparation of metal sulfide quantum dots: add metal chloride to oleic acid to prepare a mixed solution of oleic acid metal chloride with a concentration of 0.1-0.5mol / L, and stir magnetically at 90-170°C for 25-35min Finally, in the oleic acid metal chloride mixed solution, add a concentration of 0.2-0.6mol / L oleic acid solution dissolved with elemental sulfur, the volume of the oleic acid metal chloride mixed solution and the oleic acid solution dissolved with elemental sulfur The ratio is 2:1, and magnetically stirred at 150-320°C for 55-65min to obtain the crude product of metal sulfide quantum dots. Add absolute ethanol to the crude product of metal sulfide quantum dots to precipitate the metal sulfide quantum dots. Centrifuge at 8000-12000 rpm, wash the precipitate with absolute ethanol for more than three times, vacuum-dry the precipitate at 45-55°C to obtain metal sulfide quantum dots, dissolve the metal sulfide quantum dots in n-hexane, and The mass of the ...

Embodiment 1

[0034] Add 2mmol of zinc chloride to 10mL of oleic acid to prepare a mixed solution of oleic acid metal chloride with a concentration of 0.2mol / L. After magnetic stirring at 170°C for 30min, add 5mL A 0.6mol / L oleic acid solution with elemental sulfur dissolved therein was magnetically stirred at 320°C for 60 minutes to obtain a crude product of metal sulfide quantum dots, and absolute ethanol was added to the crude product of metal sulfide quantum dots to make the metal sulfide quantum dots Spot the precipitate, centrifuge at 10000rpm, wash the precipitate with absolute ethanol for more than three times, and vacuum dry the precipitate at 50°C to obtain a white solid that is zinc sulfide quantum dots. Dissolve 4.85mg of zinc sulfide quantum dots in 9.7mL In n-hexane, zinc sulfide quantum dot n-hexane solution was obtained as the oil phase of the interface reaction; another nitric acid solution with a concentration of 0.05mol / L was prepared as the water phase of the interface re...

Embodiment 2

[0037] Add 5mmol of manganese chloride to 10mL of oleic acid to prepare a mixed solution of oleic acid metal chloride with a concentration of 0.5mol / L. After magnetically stirring at 120°C for 25min, add 5mL A 0.2mol / L oleic acid solution with elemental sulfur dissolved therein was magnetically stirred at 280°C for 55 minutes to obtain the crude product of metal sulfide quantum dots, and absolute ethanol was added to the crude product of metal sulfide quantum dots to make the metal sulfide quantum dots Spot the precipitate, centrifuge at 8000rpm, wash the precipitate with absolute ethanol for more than three times, and vacuum-dry the precipitate at 45°C to obtain a black solid that is manganese sulfide quantum dots. Dissolve 26.1mg of manganese sulfide quantum dots in 78.3mL In n-hexane, manganese sulfide quantum dot n-hexane solution was obtained as the oil phase of the interfacial reaction; another nitric acid solution with a concentration of 0.04mol / L was prepared as the aqu...

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Abstract

The invention discloses a technology for synthesizing sulfur quantum dots through an oil-water interface method. The technology comprises the following steps: 1, preparing metal sulfide quantum dots; 2, preparing a nitric acid solution; and 3, preparing sulfide quantum dots. In the invention, oleic acid is used as a solvent to prepare oil-soluble metal sulfide quantum dots, an n-hexane solution of a metal sulfide and an aqueous solution of nitric acid are mixed as an oil phase and a water phase respectively, nitric acid oxidizes sulfide ions into elemental sulfur in situ at the phase interface, and the metal sulfide quantum dots are adopted as a template to realize the uniform distribution of the particle sizes of the prepared sulfur quantum dots, so the oil-water interface alleviates the reaction speed and realizes the dispersion and small particle sizes of sulfur nano-particles. The technology allows the sulfur quantum dots to be synthesized by adopting the above technical scheme through the oil-water interface reaction with the n-hexane solution of the metal sulfide as the oil phase and the aqueous solution of nitric acid as the water phase, so the technology has the advantages of mild reaction conditions, simple operation, controllable particle size and easy popularization.

Description

technical field [0001] The invention belongs to the technical field of nanometer material preparation, in particular to a method for synthesizing sulfur quantum dots by an oil-water interface method. Background technique [0002] Quantum dots (Quantum dots) are composed of a limited number of atoms, quasi-zero-dimensional nanomaterials with three dimensions smaller than 10nm. Compared with other nanomaterials, the movement of internal electrons in all directions is restricted, so quantum confinement The quantum confinement effect is particularly significant. As a new type of semiconductor fluorescent nanomaterial, it has many excellent properties due to the surface effect, dielectric effect and quantum effect caused by its special nanostructure. Sensors and other fields can be applied and developed. [0003] Sulfur is the main component of sulfur in traditional Chinese medicine, which is commonly used to treat skin diseases such as scabies, tinea capitis, acne, seborrheic ...

Claims

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Application Information

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IPC IPC(8): C01B17/06B82Y30/00
Inventor 李顺兴郑凤英陈德建
Owner MINNAN NORMAL UNIV
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