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Method for simply and massively preparing graphene dispersed molybdenum base sulfide catalyst

A graphene and sulfide technology, applied in organic compound/hydride/coordination complex catalysts, physical/chemical process catalysts, chemical instruments and methods, etc. Low-cost, wide-ranging, and simple-to-method effects

Inactive Publication Date: 2015-03-18
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

However, there is still a certain gap in the efficiency of this type of catalyst for electrolyzing water compared with platinum. In addition, the method of obtaining this type of catalyst often requires an ultra-high vacuum process (I. Chorkendorff et al., Science317, 100 (2007)) , or require high temperature treatment (H.J.Dai et al., J.Am.Chem.Soc.133, 7296 (2011)), or the vulcanization process requires the use of toxic gas H 2 S (T.F.Jaramillo et al., Nano.Lett.11, 4168(2011)), these complex processes restrict the simple and macro preparation of this type of catalyst

Method used

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  • Method for simply and massively preparing graphene dispersed molybdenum base sulfide catalyst
  • Method for simply and massively preparing graphene dispersed molybdenum base sulfide catalyst
  • Method for simply and massively preparing graphene dispersed molybdenum base sulfide catalyst

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] 1. Seal 60g of ball milling balls (stainless steel balls, 1.2cm in diameter), 0.32g of graphene, 0.68g of ammonium tetrathiomolybdate, and 20ml of hydrazine hydrate into a ball milling tank under argon protection.

[0033] 2. Put the ball mill jar in (1) on a ball mill and mill it at a speed of 450 rpm for 20 hours.

[0034] 3. Take out the ball milling ball with tweezers, filter the sample with suction, and dry the sample in an oven at 100°C to obtain the catalyst.

[0035] 0.65g of catalyst can be prepared in one time. X-ray diffraction spectrum (see figure 1 ) shows that the diffraction peak distribution of the molybdenum-based sulfide in the obtained catalyst is wider, indicating that the obtained molybdenum-based sulfide is more dispersed. X-ray photoelectron spectroscopy (see figure 2 ) shows that the prepared catalyst contains mainly C, N, O, S, Mo, and the valence state of Mo element is +4 valence and +6 valence.

Embodiment 2

[0037] 1. Seal 60g of ball milling balls (zirconia balls, 0.2cm in diameter), 0.32g of nitrogen-doped graphene, 0.68g of ammonium tetrathiomolybdate, and 10ml of hydrazine hydrate into a ball milling jar under argon protection.

[0038] 2. Put the ball mill jar in (1) on a ball mill and mill at a speed of 500 rpm for 10 hours.

[0039] 3. Separate the balls from the sample through a sieve, filter the sample with suction, and dry the sample in an oven at 120°C to obtain the catalyst.

[0040] About 0.6g of catalyst can be prepared in a single tank. The X-ray diffraction spectrum shows that the molybdenum-based sulfides in the obtained catalyst are relatively dispersed. X-ray photoelectron spectroscopy showed that the valence state of Mo element in the prepared catalyst was +4 and +6.

Embodiment 3

[0042] 1. Seal 180g of ball milling balls (zirconia balls, 0.8cm in diameter), 0.64g of boron-doped graphene, 1.36g of ammonium polythiomolybdate, and 5ml of ammonia water into a ball milling jar under nitrogen protection.

[0043] 2. Put the ball mill jar in (1) on a ball mill and mill at a speed of 600 rpm for 10 hours.

[0044] 3. Separate the ball milling balls from the sample through a sieve, and filter with suction. The catalyst was obtained by drying the sample in an oven at 150°C.

[0045] About 1.5g of catalyst can be prepared in a single tank. The X-ray diffraction spectrum shows that the molybdenum-based sulfides in the obtained catalyst are relatively dispersed. X-ray photoelectron spectroscopy showed that the valence state of Mo element in the prepared catalyst was +4 and +6.

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Abstract

The invention discloses a method for simply and massively preparing a graphene dispersed molybdenum base sulfide catalyst. The method is characterized in that the catalyst is obtained in one step through direct ball milling of graphene, a molybdenum base sulfide precursor and a reducing agent, and the activity of the catalyst can be effectively adjusted by changing the ratio among raw materials, the ball milling time, the rotating speed and energy. The method has the characteristics of simplicity, easy operation and control, and convenient and fast realization of large scale production.

Description

technical field [0001] The invention relates to a method for simple and large-scale preparation of graphene-dispersed molybdenum-based sulfide catalysts. Background technique [0002] With the continuous exploitation and consumption of fossil fuels, the reserves of global fossil fuels are getting less and less, and the energy crisis is getting more and more serious. At the same time, greenhouse gases and other toxic and harmful gases emitted by fossil fuel combustion have also caused serious damage to the ecological environment. Therefore, it is particularly important to find a clean and renewable energy source, and hydrogen energy has attracted widespread attention, which makes how to efficiently obtain hydrogen an important topic of current research. At present, the large-scale acquisition of hydrogen is mainly through the steam reforming of methane, but methane is a non-renewable resource, and the carbon dioxide produced by reforming will bring about a series of problems...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24B01J31/02
Inventor 包信和邓浇邓德会
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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