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Method for preparation of hollow molybdenum disulfide microspheres in inverse microemulsion

A technology of inverse microemulsion and molybdenum disulfide, which is applied in the direction of molybdenum sulfide, etc.

Inactive Publication Date: 2018-05-29
PETROCHINA CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Currently using MoCl 5 As a raw material, hollow MoS was prepared by one-step microemulsion hydrothermal treatment 2 Microsphere structure has not been reported yet

Method used

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  • Method for preparation of hollow molybdenum disulfide microspheres in inverse microemulsion
  • Method for preparation of hollow molybdenum disulfide microspheres in inverse microemulsion
  • Method for preparation of hollow molybdenum disulfide microspheres in inverse microemulsion

Examples

Experimental program
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Effect test

Embodiment 1

[0026] Mix 30g TritonX-100, 15g n-pentanol, and 150g cyclohexane evenly under 14000rpm mechanical stirring to obtain a uniform and transparent solution, which is marked as mixture A, divided into 3 parts and set aside; win the prize in a glove box filled with nitrogen atmosphere 1.85gMoCl 5 Add the powder to a portion of mixture A; 500rpm electromagnetic stirring is uniform, and the resulting solution is marked as mixture B; take a portion of mixture A, add 5.5mL of 2.5mol / L ammonium sulfide solution under stirring at 14000rpm, and continue stirring for 5min to obtain an inverse microemulsion C; take a portion of mixture A, add 1mL of 16mol / L hydrazine hydrate solution under stirring at 14000rpm, and continue stirring for 5 minutes to obtain mixture D; under stirring at 14000rpm, slowly mix solutions B, C, and D, and continue stirring for 10 minutes to obtain micro Emulsion E, transfer 50mL microemulsion to a 100mL stainless steel reaction kettle with polytetrafluoroethylene lin...

Embodiment 2

[0029] Mix 30g TritonX-100, 15g n-pentanol, and 150g cyclohexane evenly under 14000rpm mechanical stirring to obtain a uniform and transparent solution, which is marked as mixture A, divided into 3 parts and set aside; win the prize in a glove box filled with nitrogen atmosphere 0.90gMoCl 5 Add the powder to a portion of mixture A; 500rpm electromagnetic stirring is uniform, and the resulting solution is marked as mixture B; take a portion of mixture A, add 5.5mL of 1.3mol / L ammonium sulfide solution under stirring at 14000rpm, and continue stirring for 5min to obtain an inverse microemulsion C; take a portion of mixture A, add 1mL 8mol / L hydrazine hydrate solution under stirring at 20000rpm, and continue stirring for 5min to obtain mixture D; under stirring at 20000rpm, slowly mix solutions B, C, and D, and continue stirring for 10min to obtain micro Emulsion E, transfer 60mL of microemulsion to a 100mL stainless steel reaction kettle with polytetrafluoroethylene lining, plac...

Embodiment 3

[0031] Mix 30g TritonX-100, 15g n-pentanol, and 150g cyclohexane evenly under 14000rpm mechanical stirring to obtain a uniform and transparent solution, which is marked as mixture A, divided into 3 parts and set aside; win the prize in a glove box filled with nitrogen atmosphere 1.85gMoCl 5 Add the powder to a portion of mixture A; 500rpm electromagnetic stirring is uniform, and the resulting solution is marked as mixture B; take a portion of mixture A, add 5.5mL of 2.5mol / L ammonium sulfide solution under stirring at 14000rpm, and continue stirring for 5min to obtain an inverse microemulsion C; take a portion of mixture A, add 1mL of 16mol / L hydrazine hydrate solution under stirring at 14000rpm, and continue stirring for 5 minutes to obtain mixture D; under stirring at 14000rpm, slowly mix solutions B, C, and D, and continue stirring for 10 minutes to obtain micro Emulsion E, transfer 50mL of microemulsion to a 100mL stainless steel reactor with polytetrafluoroethylene liner,...

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Abstract

The invention provides a method for preparation of hollow molybdenum disulfide microspheres in an inverse microemulsion. The method mainly includes the steps of: (1) mixing polyethylene glycol octylphenyl ether (Triton X-100), alcohol and cyclohexane evenly to obtain a mixture A, and dividing the mixture A equally into three parts for standby use; in an inert atmosphere, dissolving MoCl5 in one part of the mixture A to obtain a solution B; adding an aqueous solution of a sulfur source and an aqueous solution of a reducing agent respectively into one part of A and performing mixing to obtain amicroemulsion C and a microemulsion D; and then mixing the B, C and D to obtain an inverse microemulsion E; and (2) placing the inverse microemulsion E in a high-pressure reaction kettle, conducting sealing, then conducting reaction at 120-250DEG C for 3-72, performing cooling, and then conducting separation, washing and drying to obtain a black powder sample, and conducting scanning electron microscope and transmission electron microscope characterization to obtain hollow molybdenum disulfide microspheres with a particle size of 100-500nm. The method provided by the invention has the advantages of simple preparation process, abundant raw materials and low cost.

Description

technical field [0001] The invention relates to a method for preparing hollow MoS in inverse microemulsion 2 microsphere method. Background technique [0002] Molybdenum disulfide is a hexagonal layered crystal with a layered structure similar to graphene, MoS 2 The single layer is an S-Mo-S sandwich structure formed by sandwiching a Mo atomic layer between two S atomic layers. The inner layer is a stronger Mo-S covalent bond, and the interlayer is a weaker van der Waals bond. force. MoS 2 It is anisotropic, easy to slip between layers, has a low friction coefficient, and the weak force between layers allows the insertion of guest molecules, and the unsaturated Mo or S atoms at the edge of the layer are catalytic for some hydrogenation reactions effect. MoS 2 Due to its special structure, it has excellent optical, electrical, magnetic, lubricating and catalytic properties, and has broad application prospects in the fields of catalytic hydrogenation, lubricants, hydroge...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G39/06
CPCC01G39/06C01P2002/85C01P2004/03C01P2004/04C01P2004/34C01P2004/62
Inventor 田志坚姜玉霞潘振栋王冬娥李鹏李佳鹤李敏
Owner PETROCHINA CO LTD
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