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A kind of preparation method of nanoscale supported molybdenum sulfide catalyst

A nano-scale, catalyst technology, applied in the direction of catalyst activation/preparation, physical/chemical process catalyst, molybdenum sulfide, etc., can solve the problem of reducing surface energy, improving the degree of dispersion and suspension, and unfavorable active sites with many stacked layers of nanosheets Exposure and other issues to achieve the effect of avoiding self-agglomeration

Active Publication Date: 2021-12-07
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

The aforementioned wet chemical synthesis of MoS 2 Materials, how many nanosheets are stacked and assembled, the size is at the level of hundreds of nanometers or even microns, and the number of stacked layers of nanosheets is not conducive to the exposure of its active sites
However, due to the MoS produced during the wet synthesis 2 Nanosheets have extremely high surface energy. During the crystallization process, they are often aggregated into micro / nanospheres, nanoflowers, hollow cages, etc. to reduce the surface energy, which undoubtedly leads to the embedding and covering of many catalytic active sites.
Furthermore, this self-agglomerated MoS 2 material, the dispersibility and suspension degree in the residual oil suspension bed hydrogenation system need to be improved

Method used

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  • A kind of preparation method of nanoscale supported molybdenum sulfide catalyst
  • A kind of preparation method of nanoscale supported molybdenum sulfide catalyst
  • A kind of preparation method of nanoscale supported molybdenum sulfide catalyst

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Experimental program
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Effect test

Embodiment 1

[0026] Disperse 7.5 mmol of commercial titanium oxide carrier in 60 ml of deionized water, and stir ultrasonically to form a suspension evenly. Dissolve 0.16mmol of ammonium molybdate and 3.48mmol of ammonium sulfide in the suspension and stir evenly so that the Mo / Ti molar ratio is 0.15. Then add 6.72mmol of hydrazine hydrate reducing agent to make Mo / reducing agent 1:6. After fully stirring, the suspension was transferred to a 100ml hydrothermal kettle, reacted at 180°C for 12h, cooled naturally to room temperature, filtered with suction, washed with deionized water and absolute ethanol, dried under vacuum at 70°C overnight, and collected nano Grade Loaded MoS 2 sample. The samples were characterized by HRTEM. HRTEM results showed that the prepared MoS2 was nanosheets with stacked layers of 2-3 layers and a sheet length of 10-20nm. The carrier used was highly dispersed nanoparticles figure 1 a).

Embodiment 2

[0028] Disperse 7.5 mmol of self-made titanium oxide carrier in 60 ml of deionized water, and stir ultrasonically to form a suspension evenly. Dissolve 2.24mmol of molybdenum oxide and 6.96mmol of sodium sulfide in the suspension and stir evenly to make the Mo / Ti molar ratio 0.3. Then add 6.72mmol of hydrazine hydrate reducing agent to make Mo / reducing agent 1:3. After fully stirring, the suspension was transferred to a 100ml hydrothermal kettle, reacted at 160°C for 24h, cooled naturally to room temperature, filtered with suction, washed with deionized water and absolute ethanol, dried under vacuum at 70°C overnight, and collected nano Grade Loaded MoS 2 sample. The samples were characterized by HRTEM. The HRTEM results showed that the prepared MoS2 was nanosheets with 2-3 stacked layers and a sheet length of 10-15nm. The carrier used was highly dispersed nanoparticles 2 The small size and low packing load maximize the exposure of its catalytic active side (see figure 1 b)...

Embodiment 3

[0030] Disperse 7.5 mmol of commercial titanium oxide carrier in 60 ml of deionized water, and stir ultrasonically to form a suspension evenly. Dissolve 0.11 mmol of ammonium tetrathiomolybdate in the suspension and stir evenly so that the Mo / Ti molar ratio is 0.015. Then add 0.66mmol of hydrazine hydrate reducing agent to make Mo / reducing agent 1:6. After fully stirring, transfer the suspension to a 100ml hydrothermal kettle, react at 200°C for 6h, cool to room temperature naturally, filter with suction, wash the precipitate with deionized water and absolute ethanol, dry it under vacuum at 70°C overnight, and collect nano Grade Loaded MoS 2 sample. The samples were characterized by HRTEM, and the HRTEM results showed that the prepared MoS 2 It is a nanosheet with a stacked layer number of 1-2 layers and a sheet length of 5-10nm. The carrier used is a highly dispersed nanoparticle of 2 The small size and low packing load maximize the exposure of its catalytic active side (s...

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Abstract

The invention discloses a nanoscale loaded molybdenum sulfide (MoS 2 ) The preparation method of the catalyst. The invention includes the following steps: disperse / dissolve a certain amount of carrier, molybdenum source and sulfur source in deionized water, and stir after ultrasonic dispersion to obtain a suspension; add an appropriate amount of reducing agent and stir evenly; regulate the molybdenum source, sulfur source and The type of carrier; place the prepared solution or suspension in a closed stainless steel reaction kettle, control the reaction temperature at 120-200°C, and the reaction time is 3-36h; after the reaction is completed, cool, filter, wash, and dry to obtain Nanoscale supported MoS 2 catalyst. The synthesis method of the present invention has the advantages of mild conditions, simple operation and high yield, and the prepared nano-scale supported MoS 2 The catalyst has high active site exposure rate and high dispersion. The method of the present invention synthesizes nanoscale loaded MoS 2 The catalyst is used in the field of oil catalytic hydrogenation with extremely high catalytic hydrogenation activity.

Description

technical field [0001] The invention relates to a nano-scale loaded MoS 2 The preparation method of the catalyst belongs to the field of controllable preparation of high-efficiency nano-catalysts 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 material and photoelectrochemic...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/051B01J37/10B01J35/02B82Y40/00C01G39/06
CPCB01J27/051B01J35/02B01J37/10B82Y40/00C01G39/06
Inventor 王冬娥田志坚李佳鹤李敏马怀军潘振栋郑安达曲炜李鹏
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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