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Micro-emulsion method for preparing nano-sulfur particles

A technology of nano-sulfur and micro-emulsion, which is applied in the field of chemistry and chemical engineering, can solve problems such as complex processes, and achieve the effects of uniform particle size distribution, adjustable particle size distribution, and simple methods

Active Publication Date: 2010-11-10
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Among the above technologies, the CVD method needs to be operated under high temperature conditions, and the process is complicated; other technical methods are carried out in the liquid phase, but the high specific surface area of ​​nanoparticles produces high specific surface energy, which makes it easy for the particles to adsorb and agglomerate to form large particles. agglomerated particles

Method used

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  • Micro-emulsion method for preparing nano-sulfur particles
  • Micro-emulsion method for preparing nano-sulfur particles
  • Micro-emulsion method for preparing nano-sulfur particles

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] After mixing 8g span80-tween80 composite surfactant (HLB: 5.5), 1ml n-butanol and 45ml n-octane for 15 minutes, add 3ml Na 2 S x(0.5mol / L) solution and stirred to obtain clear microemulsion A in 15 minutes. Prepare clear microemulsion B containing 3ml HCl (1mol / L) solution in the same way (that is, after mixing 8g span80-tween80 composite surfactant (HLB: 5.5), 1ml n-butanol and 45ml n-octane for 15 minutes, add 3ml HCl (1mol / L) solution and stirred for 15 minutes to obtain a clear microemulsion B). Then microemulsion A and microemulsion B were mixed and stirred for 30 minutes, then aged for 12 hours, then a certain amount of acetone was added and stirred to obtain a precipitate, and the precipitate was alternately washed with deionized water and acetone under suction filtration conditions to remove the oil phase and surface activity agent, and then dried under vacuum at 50°C for 12 hours to obtain the product sulfur particles. The particle size range of gained produ...

Embodiment 2

[0039] After mixing 4g tween80, 0.5ml n-butanol and 20ml n-octane for 15 minutes, add 1ml Na 2 S x (0.5mol / L) solution and stirred for 15 minutes to obtain clear microemulsion A; prepare clear microemulsion B containing 1ml HCl (1mol / L) solution with the same method. Then the product sulfur particles were obtained according to the method of Example 1. The particle size range of the obtained product sulfur is shown in Table 1. The detection by transmission electron microscope and XRD proves that the particle size distribution of the obtained nano-sulfur is uniform, there is no agglomeration phenomenon, and it is an orthorhombic crystal system without impurity phases.

Embodiment 3

[0041] Stir 2g of cetyltrimethylammonium bromide (CTAB), 2ml of n-butanol and 30ml of n-octane for 15 minutes to make them evenly mixed, then add 2ml of Na 2 S x (0.5mol / L) solution and stirred for 30 minutes to clear microemulsion A; the same method was prepared to obtain clear microemulsion B containing 2ml HCl (1mol / L) solution. Then obtain sulfur particles according to the method of Example 1. The particle size range of gained product sulfur is shown in Table 1, and its transmission electron microscope figure is as follows image 3 shown. The detection by transmission electron microscope and XRD proves that the particle size distribution of the obtained nano-sulfur is uniform, there is no agglomeration phenomenon, and it is an orthorhombic crystal system without impurity phases.

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Abstract

The invention relates to a method for preparing nano particles of elemental sulfur, belonging to the technical filed of chemistry and chemical industry. In the invention, a micro-emulsion method is utilized to prepare nano-sulfur particles and comprises the following steps: (1) evenly mixing surfactant, cosurfactant and oil phase, adding water solution of sulfur precursor to form micro-emulsion A, wherein the sulfur precursor is a compound capable of performing dismutation under acidic condition to generate the elemental sulfur; (2) evenly the mixing surfactant, the cosurfactant and the oil phase, then adding aqueous acid to form micro-emulsion B; and (3) mixing the micro-emulsion A obtained in step (1) and micro-emulsion B obtained in step (2), after the reaction ends, ageing, breaking emulsion, separating, washing and drying to obtain the nano-sulfur particles. The obtained product is orthorhombic system elemental sulfur, contains no impurity phase, and has evenly particle diameter distribution; and the particle diameter ranges from 10 to 400nm.

Description

technical field [0001] The invention relates to a method for preparing sulfur nanoparticles. It belongs to the field of chemical engineering. Background technique [0002] Sulfur is an element with abundant reserves. The main form of sulfur in nature is pyrite, sulfate or elemental state. Sulfur is widely used in biomedicine, chemistry, energy and other fields. For example, in terms of chemical power sources, sodium-sulfur batteries and lithium-sulfur batteries directly use elemental sulfur as the positive electrode active material of batteries. Sulfur has its unique advantages as a positive electrode material: no pollution, abundant reserves, and the theoretical specific capacity of the Li / S reaction pair is 1675mAh / g, which is the material with the highest specific capacity among the known lithium battery positive electrode materials. As we all know, sulfur is an insulator, and when used as an electrode material, conductive components need to be added. The morphology of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B17/06
Inventor 温兆银梁宵刘宇张浩吴梅芬
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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