Method for preparing nano sulfur materials with different shapes based on H2O2 regulation

A technology of H2O2 and nano-sulfur, applied in the field of sulfur nanomaterials, can solve the problem of less research on the preparation method of layered sulfur nanosheets and sulfur nanorods, and achieve good multi-band PL emission characteristics, good stability, and easy availability of raw materials. Effect

Active Publication Date: 2020-07-17
XIAN UNIV OF SCI & TECH
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

Moreover, there are few studies on the preparation methods of layered sulfur nanosheets and sulfur nanorods.

Method used

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  • Method for preparing nano sulfur materials with different shapes based on H2O2 regulation
  • Method for preparing nano sulfur materials with different shapes based on H2O2 regulation
  • Method for preparing nano sulfur materials with different shapes based on H2O2 regulation

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Effect test

Embodiment 1

[0036] Embodiment 1 prepares nano-sulfur flakes

[0037] 1) Treat 3.4g of sublimated sulfur powder with nitric acid at 65°C for 54h, centrifuge and wash the precipitate four times; place the precipitate in a round bottom flask, add 50mL of deionized water and 6mL of polyethylene glycol PEG-600 at room temperature Stir for 40min to obtain a yellow suspension;

[0038] 2) Add 4.5 g of solid KOH to the yellow suspension mixture, stir at 85°C for 56 hours, the sulfur powder in the yellow suspension mixture is gradually dissolved by heating until the yellow suspension mixture turns into a red mixture;

[0039] 3) Cool the red mixture to room temperature; take 15mL of the red mixture, add 9mol / L, 2.3mL of H 2 o 2 While stirring, it can be observed that the red mixture turns into a light yellow transparent solution;

[0040] 4) Transfer the obtained light yellow transparent solution to a 100mL polytetrafluoroethylene reactor, and keep it in an oven at a temperature of 170° C. for ...

Embodiment 2

[0042] Embodiment 2 prepares nano-sulfur flakes

[0043] 1) Treat 1.4g of sublimated sulfur powder with nitric acid at 70°C for 48h, centrifuge and wash the precipitate three times; place the precipitate in a round bottom flask, add 50mL of deionized water and 4mL of polyethylene glycol PEG-400, at room temperature Stir for 30min to obtain a yellow suspension mixture;

[0044] 2) Add 4 g of solid NaOH to the yellow suspension mixture, stir at 70°C for 24 hours, the sulfur powder in the yellow suspension mixture is gradually dissolved by heating until the yellow suspension mixture turns into a red mixture;

[0045] 3) Cool the red mixture to room temperature; take 15mL of the red mixture, add 9.8mol / L, 2.1mL of H 2 o 2 , while stirring, it can be observed that the red mixed solution turns into a light yellow transparent solution;

[0046] 4) Transfer the obtained light yellow transparent solution to a 100 ml polytetrafluoroethylene reaction kettle, and keep it in an oven at ...

Embodiment 3

[0047] Embodiment 3 prepares nano-sulfur flakes

[0048] 1) Treat 1.0g of sublimated sulfur powder with nitric acid at 80°C for 40h, centrifuge and wash the precipitate three times; place the precipitate in a round bottom flask, add 50mL of deionized water and 6mL of polyethylene glycol PEG-200, at room temperature Stir for 25min to obtain a yellow suspension;

[0049] 2) Add 3.5 g of solid NaOH to the yellow suspension mixture, stir at 60°C for 72 hours, the sulfur powder in the yellow suspension mixture is gradually dissolved by heating until the yellow suspension mixture turns into a red mixture;

[0050] 3) Cool the red mixture to room temperature; take 15mL of the red mixture and add 10mol / LH dropwise to it 2 o 2 1.8mL, while stirring, it can be observed that the red mixture turns into a light yellow transparent solution;

[0051] 4) The obtained light yellow transparent solution was transferred to a 100 ml polytetrafluoroethylene reactor, and kept in an oven at a temper...

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Abstract

The invention belongs to the technical field of sulfur nano materials, and relates to a method for preparing nano sulfur materials with different shapes based on H2O2 regulation, which comprises the following steps: 1) treating sublimed sulfur powder with nitric acid, and centrifugally washing; adding the precipitate and PEG into water, and stirring to obtain a yellow suspension mixed solution; 2)adding solid alkali into the yellow mixed solution until the yellow mixed solution becomes a red mixed solution, and cooling to room temperature; 3) adding H2O2 into the cooled red mixed solution, and stirring to change the red mixed solution into a faint yellow transparent solution; and 4) putting the faint yellow transparent solution into a reaction kettle to obtain the layered or rod-like nanosulfur material. According to the invention, different amounts of H2O2 are added; the novel layered nano sulfur and the nano sulfur rod are directly prepared in a reaction kettle, meanwhile, the layered nano sulfur is subjected to ultrasonic treatment to obtain the nano sulfur sheet, the operation method is simple, and the sulfur nano sheet has good water dispersibility, multiband PL emission characteristics and electrochemical properties and obvious optical absorption characteristics.

Description

technical field [0001] The invention belongs to the technical field of sulfur nanomaterials, and relates to a 2 o 2 Controlling the method of preparing nano-sulfur materials with different shapes. Background technique [0002] In recent years, in addition to graphene, molybdenum disulfide and black phosphorus (BP) have also been prepared, greatly expanding the performance and application of two-dimensional materials; however, BP is unstable in air, and its surface is exposed to air After 24 hours, bubbles will be generated and oxidative degradation will occur; in addition, its preparation difficulty is also a bottleneck that limits its further application; at the same time, in multilayer molybdenum disulfide, the indirect band gap greatly reduces the photoluminescence (PL) efficiency and photoelectric conversion efficiency , so that the optoelectronic application of multilayer molybdenum disulfide is greatly restricted. [0003] In order to solve these problems, researche...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/02B01J35/02B82Y30/00B82Y40/00
CPCB01J27/02B01J35/004B01J35/023B01J35/0033B82Y30/00B82Y40/00Y02E60/10
Inventor 申丽华陈小倩白状伟魏建航于春侠
Owner XIAN UNIV OF SCI & TECH
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