Preparation method and application of copper sulphide/molybdenum sulfide composite

A composite material and molybdenum sulfide technology, applied in catalyst activation/preparation, chemical instruments and methods, hydrogenation hydrocarbon production, etc., can solve the problems of low purity of molybdenum disulfide, harsh reaction conditions, high economic cost, etc., to avoid post-processing The effect of simplification of steps and preparation process and simple operation process

Active Publication Date: 2019-04-05
DONGGUAN UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, the preparation methods of molybdenum disulfide are as follows: hydrothermal or solvothermal method, thermal decomposition method, chemical vapor deposition method, microwave method, mechanical stripping method, template method, electrochemical method, etc., the above preparation methods are currently available To a certain extent, the morphology and size of molybdenum disulfide are controlled, and the preparation method of molybdenum disulfide is optimized; although there are many methods found now, there are still many problems, such as harsh reaction conditions, complicated equipment, and the formation of molybdenum disulfide. Therefore, it is urgent to develop a synthesis method with mild reaction conditions, simple operation, high repeatability, low cost, and activation of a large number of inert substrates to prepare copper sulfide with excellent catalytic activity. / Molybdenum sulfide composites are of great significance

Method used

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  • Preparation method and application of copper sulphide/molybdenum sulfide composite
  • Preparation method and application of copper sulphide/molybdenum sulfide composite
  • Preparation method and application of copper sulphide/molybdenum sulfide composite

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Experimental program
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Effect test

Embodiment 1

[0029] Under the protection of nitrogen, the ratio of molybdenum, copper and sulfur is 1:A:2.5 (NH 4 ) 6 Mo 7 O 24 ·4H 2 O, Cu(CH 3 COO) 2 With 1,3-two (thioacetic acid-S-n-propyl) imidazolium bromide and 50ml water join successively in volume is 100mL reactor, described (NH 4 ) 6 Mo 7 O 24 ·4H 2 The mass concentration of O was 5 mg / mL, the mixed solution was stirred for 30 minutes, then the reaction kettle was placed in an oven, and the reaction was carried out at 160 ° C for 8 hours. Centrifuge for 5 minutes, wash the powder obtained after centrifugation with methanol and distilled water for 3 times in turn, filter, and then place it in a vacuum drying box with a vacuum degree of -1Mpa and vacuum dry it at 40 ° C for 12 hours. Catalytically active copper sulfide / molybdenum sulfide composites for hydrogen production from water electrolysis.

[0030] The copper sulfide / molybdenum sulfide composites prepared with different molybdenum and copper content ratios were su...

Embodiment 2

[0038] Under nitrogen protection, the ratio of molybdenum, copper, and sulfur is 1:1:2.5 (NH 4 ) 6 Mo 7 O 24 ·4H 2 O, Cu(CH 3 COO) 2 With 1,3-two (thioacetic acid-S-n-propyl) imidazolium bromide and 50ml water join successively in volume is 100mL reactor, described (NH 4 ) 6 Mo 7 O 24 ·4H 2 The mass concentration of O was 5 mg / mL, the mixed solution was stirred for 30 minutes, then the reaction kettle was placed in an oven, and the reaction was carried out at 120-200 ° C for 8 hours. centrifugation for 5 min, the powder obtained after centrifugation was washed 3 times with methanol and distilled water in turn, filtered, and then placed in a vacuum drying box with a vacuum degree of -1Mpa and vacuum-dried at 40°C for 12 hours to obtain Copper sulfide / molybdenum sulfide composites with excellent catalytic activity for hydrogen production from water electrolysis.

[0039] The copper sulfide / molybdenum sulfide composites prepared at different reaction temperatures were ...

Embodiment 3

[0045] Under nitrogen protection, the ratio of molybdenum, copper, and sulfur is 1:1:2.5 (NH 4 ) 6 Mo 7 O 24 ·4H 2 O, Cu(CH 3 COO) 2 With 1,3-two (thioacetic acid-S-n-propyl) imidazolium bromide and 50ml water join successively in volume is 100mL reactor, described (NH 4 ) 6 Mo 7 O 24 ·4H 2 The mass concentration of O was 5 mg / mL, the mixed solution was stirred for 30 minutes, then the reaction kettle was placed in an oven, and the reaction was carried out at 160 ° C for 2 to 16 hours, and then the reaction kettle was naturally cooled to room temperature, and the mixture was taken out at 8000 r centrifugation for 5 min, the powder obtained after centrifugation was washed 3 times with methanol and distilled water in turn, filtered, and then placed in a vacuum drying box with a vacuum degree of -1Mpa and vacuum-dried at 40°C for 12 hours to obtain Copper sulfide / molybdenum sulfide composites with excellent catalytic activity for hydrogen production from water electroly...

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Abstract

The invention discloses a preparation method and application of a copper sulphide / molybdenum sulfide composite. According to the preparation method, raw materials, namely (NH4)6Mo7O24.4H2O, Cu(CH3COO)2 and 1,3-di(thioacetic acid-S-n-propyl)imidazolium bromide are subjected to one-pot synthesis by a hydrothermal process to obtain the copper sulphide / molybdenum sulfide composite; preparation condition of the composite is evaluated according to the catalytic hydrogenation effect to naphthalene, and reaction temperature and time and proportion of raw materials in preparation of the composite are optimized; particularly, on the optimized reaction conditions that the mass ratio of Mo, Cu to S of (NH4)6Mo7O24.4H2O, Cu(CH3COO)2 and 1,3-di(thioacetic acid-S-n-propyl)imidazolium bromide is 1:1: 2.5,the reaction temperature is 160 DEG C and the reaction time is 8 hours, the catalytic hydrogenation conversion rate of the copper sulphide / molybdenum sulfide composite prepared by the method to naphthalene is up to 55.6%. In the reaction process, 1,3-di(thioacetic acid-S-n-propyl)imidazolium bromide functional ionic liquid can serve as not only a sulfur source but a surfactant, and thus use of raw materials and cost are both reduced.

Description

technical field [0001] The invention relates to the technical field of preparation methods of two-dimensional molybdenum disulfide, in particular to a preparation method and application of a copper sulfide / molybdenum sulfide composite material. Background technique [0002] With the research and development of various nanomaterials, the preparation and application of molybdenum disulfide nanomaterials have gradually entered the field of vision of scientists. In 1995, Israeli scientist R. Tenne et al. synthesized molybdenum disulfide nanomaterials with fullerene structure for the first time. After particles and nanotubes, nanorods, nanoflowers, nanowires and nanosheets of molybdenum disulfide have gradually become the research hotspots in the scientific community; in the early stage of research on molybdenum disulfide nanomaterials, due to the good friction Therefore, the material has been developed into various excellent lubricants and is widely used in the industrial field;...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/051B01J37/04B01J37/10C07C5/10C07C5/11C07C13/50C07C13/48
CPCC07C5/10C07C5/11B01J27/051B01J37/04B01J37/10C07C2602/28C07C2527/051C07C13/50C07C13/48
Inventor 徐红娇马浩鹏
Owner DONGGUAN UNIV OF TECH
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