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Method for hydro-thermally synthesizing MoS<2> nanoflower with sulfur-containing biological reagent as sulfur source

A biological reagent, hydrothermal synthesis technology, applied in nanotechnology, nanotechnology, nanotechnology, etc. for materials and surface science, can solve problems such as no public reports, achieve high chemical activity, simple separation and purification, and adsorption Powerful and transparent effect

Active Publication Date: 2016-03-02
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, L-cysteine ​​and glutathione are used as sulfur sources to prepare MoS 2 The systematic study of nanoflowers has not been reported publicly

Method used

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  • Method for hydro-thermally synthesizing MoS&lt;2&gt; nanoflower with sulfur-containing biological reagent as sulfur source
  • Method for hydro-thermally synthesizing MoS&lt;2&gt; nanoflower with sulfur-containing biological reagent as sulfur source
  • Method for hydro-thermally synthesizing MoS&lt;2&gt; nanoflower with sulfur-containing biological reagent as sulfur source

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024]Weigh 1.5mmol of sodium molybdate, stir and dissolve it in 50ml of deionized water to form a 0.03M solution; add 3mmol of glutathione under stirring, and the pH of the resulting solution is 3; after fully stirring, transfer the solution to 100ml In a hydrothermal reaction kettle, conduct a hydrothermal reaction at 180°C for 18 hours. After natural cooling, filter with suction, wash the precipitate with deionized water and absolute ethanol, and then dry it under vacuum at 70°C overnight to obtain a black powder sample. XRD characterization results show that the obtained product is MoS 2 ;SEM characterization shows that the product is nanoscale MoS 2 The flower-like structure is formed by the accumulation of lamellar structure, and the dispersion is good.

Embodiment 2

[0026] Weigh 0.22mmol of ammonium molybdate, stir and dissolve it in 50ml of deionized water to form a 0.0044M solution; add 4.62mmol of L-cysteine ​​while stirring, and the pH of the resulting solution is 6; Transfer to a 100ml hydrothermal reaction kettle, and conduct a hydrothermal reaction at 200°C for 24 hours. After natural cooling, filter with suction, wash the precipitate with deionized water and absolute ethanol, and then dry it under vacuum at 70°C overnight to obtain a black powder sample. XRD characterization results show that the obtained product is MoS2; SEM characterization shows MoS 2 The surface of the microsphere is composed of a large number of sheet structures assembled in all directions, and each MoS 2 The size of the nanoflowers is about 300nm, which is different from the products prepared by common sulfur sources ( Figure 4 ) is better dispersed than ( figure 1 a); TEM characterization results show that the product is formed by cross-linking and stack...

Embodiment 3

[0028] Weigh 0.22mmol of ammonium molybdate, stir and dissolve it in 50ml deionized water to form a 0.0044M solution; add 4.62mmol of L-cysteine ​​while stirring; adjust the pH of the solution with concentrated hydrochloric acid with a mass concentration of 37.5% 1, the color of the solution changed from bright yellow to lake blue during this process; after fully stirring, the solution was transferred to a 100ml hydrothermal reaction kettle, and hydrothermally reacted at 200°C for 24 hours. After natural cooling, suction filtration was used to precipitate Washed with ionic water and absolute ethanol, and then dried under vacuum at 70 °C overnight to obtain a black powder sample. XRD characterization results show that the obtained product is MoS 2 ;SEM characterization shows that the product is about 100nm MoS 2 Nanoflowers are formed by stacking lamellar structures with good dispersion ( figure 2 ).

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Abstract

The invention discloses a method for hydro-thermally synthesizing a MoS<2> nanoflower with a sulfur-containing biological reagent as a sulfur source. The method comprises the following steps of adding molybdate and L-cysteine or glutathione to deionized water separately for forming a uniform solution, wherein the concentration of the molybdate is 0.002-0.03 M, the mole ratio of S to Mo in raw materials is 4 to 1-2 to 1, and adjusting the pH value of the solution to be 1-7 with hydrochloric acid or ammonia water; shifting the compounded solution to a hydro-thermal reaction kettle with the volume being 100 ml for seal, and conducting a hydro-thermal reaction for 18-36 hours at the temperature of 180-220 DEG C; after the solution is cooled naturally, conducting suction filtration, washing and drying, and obtaining the MoS<2> nanoflower with slice layers accumulated and the surface rough. A MoS<2> product synthesized through the method is at the nanoscale in dimension, is good in dispersion property and has wide application on the aspects of electrode materials, solid lubricant and particularly oil product hydrogenation catalysis.

Description

technical field [0001] The invention belongs to the field of synthesis of inorganic nanomaterials, in particular to a hydrothermal synthesis of MoS using sulfur-containing biological reagents as sulfur sources 2 The nanoflower approach. technical background [0002] MoS 2 It is a typical layered structure: two layers of S atoms sandwich a layer of Mo atoms to form a "sandwich" sandwich structure, and there is a weak van der Waals force between layers. The active site of its catalytic hydrogenation reaction is MoS 2 Sulfur vacancies at the edge. The traditional catalyst is bulk MoS 2 Particles are characterized by large particle size, small specific surface area, and low utilization rate of active components. Preparation of Nanoscale MoS 2 The catalyst can greatly increase the number of edge sites and improve the hydrogenation activity. In addition, nano-MoS 2 with common size MoS 2 In comparison, its anti-friction, anti-wear, fuel economy and extreme pressure proper...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G39/06B82Y30/00B82Y40/00
Inventor 田志坚李佳鹤王冬娥姜玉霞李敏潘振栋马怀军徐仁顺王从新
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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