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A method of preparing molybdenum disulfide microspheres in a reversed-phase microemulsion system

An inverse microemulsion and molybdenum disulfide technology, applied in the direction of molybdenum sulfide, etc., can solve problems such as complex operation, and achieve the effect of simple experimental equipment, controllable particle size and uniform size

Active Publication Date: 2016-07-06
PETROCHINA CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Preparation of MoS by microemulsion method 2 It is completed by two-step method, which requires pretreatment such as reduction and sulfidation of the molybdate precursor or high-temperature reduction treatment of the product, and the operation is more complicated.

Method used

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  • A method of preparing molybdenum disulfide microspheres in a reversed-phase microemulsion system
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  • A method of preparing molybdenum disulfide microspheres in a reversed-phase microemulsion system

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Experimental program
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Effect test

Embodiment 1

[0029] Polyethylene glycol octylphenyl ether (TritonX-100), n-hexanol and cyclohexane were formulated into mixture A, wherein TritonX-100 was 58.75 g, n-hexanol was 48.61 g, and cyclohexane was 79.92 g. Add 6.55 mL of 0.15 mol / L ammonium tetrathiomolybdate aqueous solution B to mixture A under stirring at 500 rpm, and stir for 30 min to form microemulsion C. Add 1.65 mL of hydrazine hydrate solution D with a concentration of 0.56 mol / L to the above microemulsion C, and stir at 500 rpm for 30 min to form microemulsion E. Transfer the microemulsion E into a hydrothermal reaction kettle, the filling volume is 60% of the free volume of the reaction kettle, seal it and stand at 180° C. for 24 hours for crystallization. Cool down to room temperature naturally after taking out the kettle. After separation by filtration, it was washed three times with deionized water and absolute ethanol to obtain a black solid product, which was dried in vacuum at 70° C. for 12 hours to obtain molyb...

Embodiment 2

[0031] Polyethylene glycol octylphenyl ether (TritonX-100), n-hexanol and cyclohexane were formulated into mixture A, wherein TritonX-100 was 58.75 g, n-hexanol was 48.61 g, and cyclohexane was 79.92 g. Add 6.55 mL of 0.15 mol / L ammonium tetrathiomolybdate aqueous solution B to mixture A under stirring at 500 rpm, and stir for 30 min to form microemulsion C. Add 1.65 mL of hydrazine hydrate solution D with a concentration of 1.4 mol / L to the microemulsion C above, and stir for 30 min to form microemulsion E. Transfer the microemulsion E into a hydrothermal reaction kettle, the filling volume is 60% of the free volume of the reaction kettle, seal it and stand at 180° C. for 24 hours for crystallization. Cool down to room temperature naturally after taking out the kettle. After separation by filtration, it was washed three times with deionized water and absolute ethanol to obtain a black solid product, which was dried in vacuum at 70° C. for 12 hours to obtain molybdenum disulf...

Embodiment 3

[0033] Polyethylene glycol octylphenyl ether (TritonX-100), n-hexanol and cyclohexane were formulated into mixture A, wherein TritonX-100 was 58.75 g, n-hexanol was 48.61 g and cyclohexane was 79.92 g. Add 6.55 mL of 0.15 mol / L ammonium tetrathiomolybdate aqueous solution B to mixture A under stirring at 500 rpm, and stir for 30 min to form microemulsion C. Add 1.65 mL of 2.24 mol / L hydrazine hydrate aqueous solution D to the microemulsion C above, and stir at 500 rpm for 30 min to form microemulsion E. Transfer the microemulsion E into a hydrothermal reaction kettle, the filling volume is 60% of the free volume of the reaction kettle, seal it and stand at 180° C. for 24 hours for crystallization. Cool down to room temperature naturally after taking out the kettle. After separation by filtration, it was washed three times with deionized water and absolute ethanol to obtain a black solid product, which was dried in vacuum at 70° C. for 12 hours to obtain molybdenum disulfide p...

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Abstract

The invention provides a method of preparing molybdenum disulfide microspheres through sulfurizing and reducing a soluble molybdenum source in a reversed-phase microemulsion system. The method includes a) a step of preparing a reversed-phase microemulsion A through adopting polyethylene glycol octylphenol ether (Triton X-100), n-hexanol, cyclohexane and an aqueous solution of the soluble molybdenum source as a surfactant, a cosurfactant, an oil phase and a water base respectively, b) a step of adding an aqueous solution containing a sulfur source and a reductant into the reversed-phase microemulsion A to obtain a reversed-phase microemulsion B, and c) a step of transferring the reversed-phase microemulsion B to a hydrothermal reactor, performing crystallization thermal treatment at a certain temperature for a certain period of time, separating, washing, and drying the reaction product to obtain the molybdenum disulfide microspheres. The method is simple and mild in reaction conditions. Through characterization by a scanning electron microscope and a transmission electron microscope, the molybdenum disulfide microspheres have the characteristics of being solid or hollow, smooth or wrinkled in surface, and the like.

Description

technical field [0001] The invention relates to a preparation method for synthesizing molybdenum disulfide microspheres in an inverse microemulsion system [0002] Law. Background technique [0003] Molybdenum disulfide is a typical transition metal sulfide, which has a layered structure similar to graphene, and each MoS 2 The layer is a sandwich structure formed by sandwiching a Mo atomic layer between two S atomic layers. The inner layer is a strong Mo-S covalent bond, and the interlayer is a weak S-S van der Waals 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. Therefore MoS 2 It has been widely used in catalytic hydrogenation, lubricants, hydrogen storage materials, lithium storage electrode materials and photochemical hydrogen producti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G39/06
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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