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Preparation method of high-activity molybdenum sulfide hydrogenation catalyst

A technology of hydrogenation catalyst and molybdenum sulfide, which is applied in the direction of catalyst activation/preparation, physical/chemical process catalysts, chemical instruments and methods, etc., and can solve the problems of no catalyst hydrogenation active site, low size accumulation degree, etc.

Inactive Publication Date: 2020-06-05
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 high-activity molybdenum sulfide hydrogenation catalyst
  • Preparation method of high-activity molybdenum sulfide hydrogenation catalyst
  • Preparation method of high-activity molybdenum sulfide hydrogenation catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Disperse 1.0g of ammonium heptamolybdate and 2.3159g of L-cysteine ​​in 60ml of glycerol, heat in a water bath to 60°C, stir to form a solution, and the S / Mo ratio is 3:1. After continuing to fully stir for 30 minutes, transfer the solution to a 100ml hydrothermal kettle, react at 180°C for 24 hours, naturally cool to room temperature, filter with suction, wash the product with deionized water and absolute ethanol, dry it under vacuum at 70°C overnight, and 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 (See figure 1 ), 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 2 and image 3 ). The two are used in the hydrogenation reaction of model...

Embodiment 2

[0030] Disperse 1.0g of ammonium heptamolybdate and 3.9166g of glutathione in 60ml of diethylene glycol, heat in a water bath to 60°C, stir to form a solution, and the S / Mo ratio is 2:1. After continuing to fully stir for 30 minutes, transfer the solution to a 100ml hydrothermal kettle, react at 140°C for 36 hours, naturally cool to room temperature, filter with suction, wash the product with deionized water and absolute ethanol, and dry it under vacuum at 70°C overnight to collect MoS 2 sample.

Embodiment 3

[0032] Disperse 0.8700g of phosphomolybdic acid and 9.5747g of thioacetamide in 60ml of a 10% mass ratio of water and glycerol mixed solution, stir to form a solution, and the S / Mo ratio is 20:1. After continuing to fully stir for 30 minutes, transfer the solution to a 100ml hydrothermal kettle, react at 220°C for 6 hours, naturally cool to room temperature, filter with suction, wash the product with deionized water and absolute ethanol, dry it under vacuum at 70°C overnight, and collect MoS 2 sample.

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Abstract

The invention discloses a preparation method of a high-activity molybdenum disulfide (MoS2) hydrogenation catalyst. The method comprises the following steps: dissolving or dispersing a certain amountof molybdenum source and reductive sulfur source in a high-viscosity solution, and adding a reducing agent to obtain a solution or turbid liquid; regulating and controlling the types of the molybdenumsource, the sulfur source and a solvent; putting the prepared solution or turbid liquid into a closed stainless steel reaction kettle, and controlling the reaction temperature to be 120-220 DEG C andthe reaction time to be 3-72 hours; and after the reaction is finished, cooling, separating, washing and drying to obtain the high-activity MoS2 hydrogenation catalyst. The synthesis method disclosedby the invention has the advantages of low temperature, low pressure, no need of adding an additional reducing agent and the like, and the prepared MoS2 hydrogenation catalyst has the advantages thatthe interlayer spacing is enlarged, the accumulation degree is less than 3 layers, and the lamellar length is shorter than 10nm, so that the highest hydrogenation active site exposure rate is achieved. The high-activity exposed nano MoS2 hydrogenation catalyst synthesized by the method disclosed by the invention has extremely high catalytic hydrogenation activity in the field of catalytic hydrogenation of oil products.

Description

technical field [0001] The invention relates to a preparation method of a highly active molybdenum sulfide hydrogenation catalyst, which belongs to the field of controllable preparation of high-efficiency nanometer catalysts and catalytic hydrogenation. Background technique [0002] MoS 2 It is a two-dimensional layered compound with semiconductor properties. Two layers of S atoms sandwich a layer of Mo atoms to form a "sandwich" sandwich structure. Mo atoms and S atoms in the layer are covalently bonded. S-Mo-S The layers are combined by weak van der Waals forces. 2H-type MoS exists stably in nature 2 : Six sulfur atoms are arranged around each Mo atom to form a triangular prism coordination structure, and there are two S-Mo-S layers stacked in each unit cell. (Ding Q. et al., Chem, 2016, 1, 699-726) Due to its unique layered structure and excellent optical, electrical and mechanical properties, MoS 2 Materials are widely used in the fields of catalysis, lubrication, op...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/051B01J37/10C10G45/16
CPCB01J27/051B01J37/10C10G45/16B01J35/23
Inventor 王冬娥田志坚马怀军曲炜韩健强王琳刘浩
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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