Molybdenum disulfide nano-catalyst preparation method, catalyst and application thereof

A nano-catalyst and molybdenum disulfide technology, which is applied in the direction of catalyst activation/preparation, physical/chemical process catalysts, chemical instruments and methods, etc., can solve problems such as poor dispersion of organic solvents, high requirements for experimental conditions, and large product sizes. Achieve the effect of improving dispersion, simple operation process and uniform size

Active Publication Date: 2017-06-09
PETROCHINA CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These schemes not only have high requirements on experimental conditions but also have relatively large size of the obtained product (generally above 200nm), serious agglomeration phenomenon,

Method used

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  • Molybdenum disulfide nano-catalyst preparation method, catalyst and application thereof
  • Molybdenum disulfide nano-catalyst preparation method, catalyst and application thereof
  • Molybdenum disulfide nano-catalyst preparation method, catalyst and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Weigh 199.6mg of ammonium thiomolybdate [(NH 4 ) 2 MoS 4 ] uniformly disperse it in 100mL of anhydrous methanol under the assistance of ultrasound, then add 380.2mg of PVP (polymerization degree = 30), and stir in a constant temperature water bath at 60°C for 0.5h, the system becomes a uniform transparent red solution . Add 1mL of hydrazine hydrate (80%) dropwise to the system, stir evenly, and transfer about 65mL into a 100mL hydrothermal reaction kettle. After sealing, the autoclave was placed in a 140°C oven. After maintaining the constant temperature for 3 hours, it was cooled naturally. The reacted product is successively washed with absolute ethanol and acetone, centrifuged three times, and vacuum-dried to obtain molybdenum disulfide nanospheres. And use it as a catalyst to evaluate its catalytic performance for anthracene hydrogenation, denoted as S1.

[0035] Depend on figure 1 , it can be found that the product obtained at a constant temperature of 140°C f...

Embodiment 2

[0038] Weigh 207mg of ammonium thiomolybdate [(NH 4 ) 2 MoS 4 ] uniformly disperse it in 100mL of anhydrous methanol under the assistance of ultrasound, then add 853mg of PVP (polymerization degree=30), after stirring in a constant temperature water bath at 60°C for 0.5h, the system becomes a uniform transparent red solution. Add 1.25 mL of hydrazine hydrate (80%) dropwise to the system, stir evenly, and then transfer about 65 mL into a 100 mL hydrothermal reaction kettle. After sealing, the kettle was placed in a 180°C oven. After maintaining the constant temperature for 3 hours, it was cooled naturally. The reacted product was successively washed with absolute ethanol and acetone, centrifuged three times, and vacuum-dried to obtain spherical nanomolybdenum disulfide, denoted as S2. Such as figure 2 .

Embodiment 3

[0040] Weigh 242mg of ammonium thiomolybdate [(NH 4 ) 2 MoS 4 ] uniformly disperse it into 100mL of anhydrous methanol under the assistance of ultrasound, then add 0.118g of PVP (polymerization degree=30), and stir in a constant temperature water bath at 60°C for 0.5h, the system becomes a uniform transparent red solution . Add 1.5 mL of hydrazine hydrate (80%) dropwise to the system, stir evenly, and then transfer about 65 mL into a 100 mL hydrothermal reaction kettle. After sealing, the kettle was placed in a 200°C oven. After maintaining the constant temperature for 3 hours, it was cooled naturally. The reacted product was successively washed with absolute ethanol and acetone, centrifuged three times, and vacuum-dried to obtain spherical nanomolybdenum disulfide, denoted as S1. Such as image 3 .

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Abstract

The invention discloses a molybdenum disulfide nano-catalyst preparation method and catalyst which can be applied to a catalytic hydrogenation process of heavy oil. According to the preparation method disclosed by the invention, ammonium tetrathiomolybdate is utilized as a raw material and a surface active agent, the ammonium tetrathiomolybdate is dissolved into absolute methanol, then a reducing agent is added after the ammonium tetrathiomolybdate is mixed evenly, and the ammonium tetrathiomolybdate is put into a constant-temperature oven of 100 to 250 DEG C to be stored for 3 to 48 hours; the molybdenum disulfide nano-catalyst can be obtained after separation. The molybdenum disulfide nano-catalyst prepared through the invention has smaller size and uniform particle size. The molybdenum disulfide nano-catalyst prepared through the invention has a larger contact angle so as to have better dispersion in organic solvent, and catalytic performance of the molybdenum disulfide nano-catalyst in a catalytic process can be improved. According to the research, the MoS2 nano-catalyst is applied to the catalytic hydrogenation process of heavy oil for the first time. Furthermore, the preparation method disclosed by the invention is simple to operate, has moderate condition, low cost and a simple synthesizing device and can be hopefully applied to industrial production.

Description

technical field [0001] The invention belongs to the technical field of preparation of molybdenum-based inorganic nanometer materials, and in particular relates to a method for preparing molybdenum disulfide nanocatalysts with uniform particle diameters. And examined its catalytic performance in the catalytic hydrogenation process of heavy oil, selected polycyclic aromatic hydrocarbon-anthracene as model object, research shows, the molybdenum disulfide nano-catalyst that the present invention prepares has higher catalytic hydrogenation process in the catalytic hydrogenation process of anthracene. Hydrogen properties. Background technique [0002] Molybdenum disulfide is a typical layered structure material, and the layers are combined by weak van der Waals force, which is easy to peel off and the layer structure is easy to control. Each molybdenum sulfide monoatomic layer is surrounded by six sulfur atoms in an octahedral (1T-MoS 2 ) or triangular prism (2H-MoS 2 ) structu...

Claims

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Application Information

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IPC IPC(8): B01J27/051B01J37/16B01J37/08C10G45/46B82Y40/00
Inventor 田志坚李敏阎立军王冬娥胡胜李佳鹤迟克彬姜玉霞李梦晨马怀军李发永潘振栋庞新梅曲炜罗琛李鹏于宏悦
Owner PETROCHINA CO LTD
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