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Method for nano sulfur atomization synthesis

A technology of nano-sulfur and chemical synthesis, applied in the preparation/purification of sulfur, etc., can solve the problems of inconvenient mass production and continuous preparation, difficult control of morphology consistency, high energy consumption, etc., to achieve good morphology consistency and increase reaction time, the effect of increasing the reaction area

Inactive Publication Date: 2015-09-30
XIAN UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to provide a nano-sulfur atomization synthesis method, which solves the difficulty of controlling the size and shape consistency of high-purity sulfur prepared by the existing supersaturated precipitation method and wet chemical precipitation method, and the inconvenience of mass production and continuous preparation problems, while avoiding the limitations of high energy consumption and high cost of the sublimation-condensation method

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  • Method for nano sulfur atomization synthesis
  • Method for nano sulfur atomization synthesis
  • Method for nano sulfur atomization synthesis

Examples

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Effect test

Embodiment 1

[0064] Starting raw material sodium thiosulfate (Na 2 S 2 o 3 ) and the hydrochloric acid whose mass fraction is 34%~36% of the precipitating agent are prepared respectively into the aqueous solution that the molar concentration is 0.01mol / L, 0.02mol / L, and the molar concentration ratio of the two is Na + :H + =1:1. Adjust the air flow of the nebulizer to 1L / min. Fill the reactor with about 250mL of buffer solution and recovery solution, start the recovery liquid flow pump and buffer solution flow pump; start the air pump to uniformly atomize the starting material solution and precipitant solution, and monitor the pH of the buffer solution at 5-6 and recovery Solution pH=12~14, after the atomization is completed, centrifuge the obtained buffer solution to obtain the nano-sulfur precipitation product, wash it with water and alcohol for 3 to 5 times until the washing solution is neutral, test for Na + Concentration ≤ 10ppm, and then drying under negative pressure at 100°C f...

Embodiment 2

[0066] The starting material sodium sulfide is dissolved in water to form a 0.25mol / L aqueous solution, and then the molar ratio of Na + : S=1: (0.8~1.5) add sublimated sulfur, stir at room temperature for 4~6h, filter the precipitate to form sodium polysulfide (Na 2 S 1 +x ) transparent solution, the mass fraction is 34% ~ 36% hydrochloric acid diluted with deionized water to obtain a 0.5mol / L precipitant solution, the molar concentration ratio of the two is Na + :H + =1:1.1. Adjust the air flow of the nebulizer to 5 L / min. Fill the reactor with an appropriate amount (the liquid level is about 15mm to 25mm) of buffer solution and recovery solution, start the recovery liquid flow pump and the buffer solution flow pump; start the air pump to uniformly atomize the starting material solution and the precipitant solution, and monitor The pH of the buffer solution is 5-6 and the pH of the recovery solution is 12-14. After the atomization is completed, the obtained buffer solut...

Embodiment 3

[0068] The starting raw material sodium sulfide is dissolved in water to form a 0.1mol / L aqueous solution, and then the molar ratio of Na + : S=1: (0.8 ~ 1.5) add sublimated sulfur, stir at room temperature for 4 ~ 6h, filter the precipitate, and form transparent sodium polysulfide (Na 2 S 1+x , x=0.7~1.4) solution, dilute formic acid with deionized water to obtain 0.2mol / L precipitant solution, the molar concentration ratio of the two is Na + :H + =1:1.2. Adjust the air flow of the nebulizer to 1.5 L / min. Fill the reactor with about 450mL of buffer solution and recovery solution, start the recovery liquid flow pump and the buffer solution flow pump; start the air pump to uniformly atomize the starting material solution and the precipitant solution, and monitor the pH of the buffer solution = 5-6 and recovery Solution pH=12~14, after the atomization is completed, the obtained buffer solution is centrifuged to obtain the nano-sulfur precipitation product, which is washed wi...

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Abstract

The invention discloses a method for nano sulfur atomization synthesis. The method concretely comprises respectively atomizing a starting material solution and a precipitant solution which are prepared well, controlling gas flow and liquid drop dimension of an atomizer, reacting to synthesize nano sulfur; scattering and precipitating the nano sulfur in a buffer solution and absorbing by-product gas phase through a recycling liquid; filtering the buffer solution through centrifugal separation to obtain nano sulfur sediment products, and performing washing and drying to obtain nano sulfur products; and evaporating and drying the remaining buffer solution and the recycling liquid to obtain reaction by-product chemical sodium salt. Through gas flow atomization, fog drips containing starting materials and fog drips containing a precipitant collide and are mixed with each other, the reaction occurs in the scale range of the fog drips; due to the limitation of the fog drip scale and concentration, the sizes of the products are far smaller than those of the fog drips, and the size uniformity and shape consistency of the obtained products are good. Reacting exhaust gas is fully absorbed through the waste gas recycling liquid and then discharged, and reacting by-products are high-purity sulphurizing salt or sulfite chemical products and are free of environmental pollution.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis of elemental sulfur, and relates to a nanometer sulfur atomization synthesis method. Background technique [0002] Represented by sublimated sulfur, my country produces about 300,000 tons of sulfur every year, which has a wide range of applications in rubber chemical industry, daily chemical industry, biomedicine and other fields. Research and application development are further broadening and subdividing the application market of high-purity sulfur. The synthesis and preparation of nano-scale high-purity sulfur is known as the current research hotspot and key technology of lithium-sulfur batteries. [0003] At present, the synthesis and preparation of nano-sulfur at home and abroad mainly include sublimation-condensation method and solution supersaturated precipitation method. The former is based on the German patent "Nanoparticles of sulfur obtained by freeze-drying aqueous sulfur dis...

Claims

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Application Information

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IPC IPC(8): C01B17/02
Inventor 张卫华游才印卢正欣洪繁
Owner XIAN UNIV OF TECH
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