Highly dispersed nano molybdenum disulfide catalyst synthetic method

A technology of nano-molybdenum disulfide and synthesis method, which is applied in the field of synthesis of highly dispersed nano-molybdenum disulfide catalyst, can solve the problem that the dispersibility of molybdenum disulfide cannot be guaranteed, the exposure of catalyst reaction active sites is affected, and the dispersibility of molybdenum disulfide is unknown. and other problems, to achieve the effect of high sphericity, short production cycle and uniform size

Inactive Publication Date: 2015-06-10
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the amount of molybdenum disulfide prepared by the electrochemical synthesis method is relatively small, and the dispersion of molybdenum disulfide after separation cannot be guaranteed.
CN102021073A discloses a preparation method for dispersing nano-molybdenum disulfide in a lubricating oil system. In the preparation process, azobisisobutyronitrile is added as an initiator, and polyvinylpyrrolidone is used as a dispersant to prepare modified nano-molybdenum disulfide Molybdenum, the molybdenum disulfide absolute ethanol solution system is dispersed in the oil solvent by using an auxiliary agent, the process is cumbersome, and the dispersibility of the molybdenum disulfide after separation is unknown
When molybdenum disulfide is used as a catalyst for hydrogenation reaction, the introduction of new substances will affect the exposure of the catalyst's reactive sites, thereby affecting the reaction activity.

Method used

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Embodiment 1

[0019] Add 0.1066-1.0660 g of self-made ammonium tetrathiomolybdate into 64 ml of diethanol solution, and continuously stir to obtain a dark red transparent solution. Add 6ml of hydrazine hydrate as reducing agent, stir to make it evenly mixed. Transfer the prepared solution to the lining of a polytetrafluorohydrothermal kettle, put it into a stainless steel hydrothermal reaction kettle and seal it, and then place the reaction kettle in an oven at 160°C for 6 hours of reaction. After the reaction is finished, cool to room temperature, transfer the reaction solution into a beaker, add an appropriate amount of acetone to settle the reaction product, remove the supernatant after precipitation, filter with suction, wash and dry to obtain a nanometer molybdenum disulfide catalyst for use.

Embodiment 2

[0021] Add 0.1773g of self-made ammonium tetrathiomolybdate into 64ml of water, methanol, ethanol or ethylene glycol solution, and continuously stir to obtain a dark red transparent solution. Add 6ml of 80% hydrazine hydrate as reducing agent, stir to mix evenly, the concentration of molybdenum source solution is 0.008mol / L. Transfer the configured solution into a polytetrafluoroethylene liner, put it into a reaction kettle and seal it, and then place the reaction kettle in an oven at 160°C for 6 hours of reaction. After the reaction is finished, cool to room temperature, transfer the reaction solution into a beaker, add an appropriate amount of acetone to settle the reaction product, remove the supernatant after precipitation, filter with suction, wash and dry to obtain a nanometer molybdenum disulfide catalyst for use.

Embodiment 3

[0023] Add 0.1773g of self-made ammonium tetrathiomolybdate into 64ml of diethanol solution, and stir continuously to obtain a dark red transparent solution. Add 6ml of hydrazine hydrate as a reducing agent, stir to make it evenly mixed, and the concentration of the molybdenum source solution is 0.008mol / L. Put the prepared solution into the polytetrafluoroethylene liner, put it into the reaction kettle and seal it, then put the reaction kettle in an oven at 120-160°C, and react for 1-12 hours. After the reaction is finished, cool to room temperature, transfer the reaction solution into a beaker, add an appropriate amount of acetone to settle the reaction product, remove the supernatant after precipitation, filter with suction, wash and dry to obtain a nanometer molybdenum disulfide catalyst for use.

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Abstract

The invention discloses a highly dispersed nano molybdenum disulfide catalyst synthetic method, homemade ammonium tetrathiomolybdate is used as a raw material, hydrazine hydrate is used as a reducing agent for solvent thermal direct preparation of a highly dispersed nano molybdenum disulfide catalyst by use of solvents of different viscosity in the solvent with special proportion, and the highly dispersed nano molybdenum disulfide catalyst has good dispersion in both organic and inorganic solvents. The molybdenum disulfide agglomeration can be inhibited by use of solvent viscosity in the solvent thermal synthetic process, so that molybdenum disulfide nanoparticles with good dispersion and uniform size can be produced. The highly dispersed nano molybdenum disulfide catalyst synthetic method has the advantages of being simple, low in cost, short in synthesis time and high in application value.

Description

technical field [0001] The invention relates to a method for synthesizing a highly dispersed nano molybdenum disulfide catalyst, which belongs to the technical field of nano catalyst preparation and dispersion. Background technique [0002] Transition group sulfides, especially molybdenum sulfides, have been used in the field of catalysis for more than 60 years. Before the Second World War, the Germans developed layered sulfide catalyst molybdenum sulfide for coal liquefaction. , because of its high activity and good anti-poisoning ability, the transition metal molybdenum sulfide MoS2 with layered structure has been used as a catalyst for hydrorefining in the petroleum industry, including hydrogenation reaction, hydrodesulfurization, oxygenation and deoxygenation, And oxygen denitrification and so on. (See Chianelli R., Catal. Today, 2009, 147, 275-286) Recently, sulfide catalysts have high reactivity and selectivity in hydrogenation reactions, so they are a class of very p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/051
Inventor 王冬娥田志坚李佳鹤李敏马怀军徐仁顺
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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