Preparation method of nano molybdenum disulfide (MoS2) hydrogenation catalyst exposed at high active site

A hydrogenation catalyst, a high-activity technology, applied in physical/chemical process catalysts, molybdenum sulfide, chemical instruments and methods, etc., can solve the problems of no catalyst hydrogenation active sites, low size and stacking degree, etc., and achieves safe synthesis conditions. The effect of increasing active site exposure and high catalytic hydrogenation activity

Active Publication Date: 2018-05-25
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the catalyst prepared by this method already has a smaller size and a lower packing degree, it does not maximize the exposure of the hydrogenation active sites of the catalyst.

Method used

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  • Preparation method of nano molybdenum disulfide (MoS2) hydrogenation catalyst exposed at high active site
  • Preparation method of nano molybdenum disulfide (MoS2) hydrogenation catalyst exposed at high active site
  • Preparation method of nano molybdenum disulfide (MoS2) hydrogenation catalyst exposed at high active site

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026]Disperse 1.62mmol of ammonium heptamolybdate and 4.25mmol of sulfur powder in 50ml of ethylene glycol to form a 0.016M molybdenum source suspension with an S / Mo ratio of 3:1. The ratio of atoms is 7:1. After ultrasonication for 10 minutes, the suspension was fully stirred and transferred to a 100ml hydrothermal kettle, reacted at 180°C for 6 hours, naturally cooled to room temperature, filtered with suction, the precipitate was washed with deionized water and absolute ethanol, and vacuum-dried at 70°C Overnight, collect MoS 2 sample. As a comparison, the commercial MoS 2 Characterization and activity evaluation were performed. The two samples were characterized by XRD and HRTEM, and it was found that the two product components were MoS 2 , but unlike commodity MoS 2 The bulk multilayer stacked structure, the MoS prepared by the present invention 2 With enlarged interlayer, lower packing degree and smaller sheet size (see figure 1 and figure 2 ). The two are use...

Embodiment 2

[0028] Disperse 5mmol of sodium molybdate and 20mmol of sodium sulfide in 50ml of ethylene glycol to form a 0.1M molybdenum source solution with a S / Mo ratio of 4:1, add 10mmol of oxalic acid to make the ratio of Mo atoms to 2:1 . After ultrasonication for 10 minutes, the suspension was fully stirred and transferred to a 100ml hydrothermal kettle, reacted at 160°C for 24 hours, cooled naturally to room temperature, filtered with suction, washed with deionized water and absolute ethanol, and dried in vacuum at 70°C Overnight, collect MoS 2 sample.

Embodiment 3

[0030] Disperse 15mmol of molybdenum oxide and 30mmol of ammonium sulfide in 50ml of diethylene glycol to form a 0.3M molybdenum source solution with an S / Mo ratio of 2:1, and add 15mmol of glucose to make the ratio of Mo atoms to 1:1. After ultrasonication for 10 minutes, the suspension was fully stirred and transferred to a 100ml hydrothermal kettle, reacted at 140°C for 48 hours, cooled naturally to room temperature, filtered with suction, washed with deionized water and absolute ethanol, and dried in vacuum at 70°C Overnight, collect MoS 2 sample.

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Abstract

The invention discloses a preparation method of a nano molybdenum disulfide (MoS2) hydrogenation catalyst exposed at a high active site. The preparation method comprises the following steps: dissolving or dispersing a certain amount of molybdenum source and sulfur source in a high-viscosity solution, and adding a reducing agent to obtain a solution or suspension liquid; adjusting and controlling the types of the molybdenum source, the sulfur source, the solvent and the reducing agent; putting the prepared solution or suspension liquid into a closed stainless steel reactor, controlling the reaction temperature to be 120-240 DEG C, and controlling the reaction time to be 3-72 hours; and after the reaction is finished, performing cooling, suction filtration, washing and drying to obtain the nano MoS2 hydrogenation catalyst exposed at the high active site. The synthetic method disclosed by the invention has the advantages of mild conditions, simple operation, high yield and the like, and the prepared nano MoS2 catalyst with expanded interlayer spacing and few layers has a high hydrogenation active site exposure rate. The nano MoS2 hydrogenation catalyst exposed at the high active site,synthesized by the method disclosed by the invention, has very high catalytic hydrogenation activity when being applied to the field of catalytic hydrogenation of oil products.

Description

technical field [0001] The invention relates to a nano-MoS with high active sites exposed 2 The preparation method of hydrogenation catalyst belongs to the field of controllable preparation of high-efficiency nanometer catalyst and catalytic hydrogenation. Background technique [0002] transition metal sulfide MoS 2 It has a typical layered structure, and the layers are combined by weak van der Waals force, which is easy to peel off. In the monoatomic layer, each molybdenum atom is surrounded by six sulfur atoms, which is in the shape of a triangular prism, exposing many Mo- The S facet can be used as a catalytic active center. (see Chianelli, R.R. Catal. Rev. 2006, 48(1), 1-41) due to MoS 2 It has the characteristics of special layered structure, anisotropy, electronic properties and noble metal-like properties. At present, the research on this material mainly focuses on catalytic hydrogenation, friction lubrication, electronic probe, hydrogen storage material, electrode...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/051B82Y30/00B82Y40/00C01G39/06C10G45/04
CPCB01J27/051B82Y30/00B82Y40/00C01G39/06C01P2002/72C01P2004/04C01P2004/64C10G45/04
Inventor 王冬娥田志坚李佳鹤李敏马怀军潘振栋王琳韩健强
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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