CN101851006A - Method for preparing MoS2 microspheres by solvent hot method - Google Patents
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Abstract
The invention relates to a method for preparing MoS2 microspheres by a solvent hot method, which comprises the following preparation steps: 1) mixing molybdenum source compounds and sulfur source compounds into an alcohol solvent, sufficiently stirring the mixture, and carrying out ultrasonic processing for sufficiently dispersing the mixture; 2) then, transferring the uniformly dispersed mixture into a reaction kettle for carrying out constant-temperature reaction; and 3) carrying out natural cooling, separation, washing and drying on reacting substances to obtain black MoS2 microspheres. The invention has the advantages of mild reaction condition, good reaction reproduction quality, simple preparation process, low preparation cost and high product yield and purity, and is hopeful to realize mass production. The MoS2 products prepared by the solvent hot method of the invention have very important application prospects in all aspects of energy storage, catalysts, solid lubricating agents and the like.
Description
[technical field]
The present invention relates to inorganic materials MoS
2Preparation field, particularly a kind of employing solvent-thermal method prepares MoS
2The method of micron ball.
[background technology]
Molybdenumdisulphide (MoS
2) be a kind of transition metal stratiform binary compound, have diamagnetism and semiconductor property, also have performances such as good light, electricity, lubricated, catalysis, enjoy people's attention always.Molybdenumdisulphide belongs to hexagonal system, and the Mo-S faceted pebble is quite a lot of, and specific surface area is big, in the layer is very strong covalent linkage, and interlayer then is more weak Van der Waals force, and layer is easy to peel off with layer, have good anisotropy and lower rubbing factor, and because S there are very strong adhesive power, MoS to metal
2Can bring into play lubricating function all the time attached to the metallic surface well, even under conditions such as high temperature, high vacuum MoS
2Still has lower rubbing factor.Though MoS
2Excellent property, but its application is subjected to the restriction of globule size, therefore need carry out super-refinement research to its preparation.
Nanometer MoS
2Comprise nanoparticle, nano-complex, nano thin-layer, soccerballene shape nanoparticle and nanotube, with common MoS
2Compare, the various performances of nano material have obtained remarkable lifting, but also have many unusual characteristics.Show the following aspects highlightedly: especially the catalytic hydrogenation desulfurization performance is stronger for catalytic performance, can be used to prepare special catalytic material and air storage material; Nanometer MoS
2Thin layer can be with the nearly 1178eV of differential, be complementary with the energy of light, on the photocell material, application prospect is arranged; Nanometer MoS
2Tack and level of coverage in friction material surface obviously improve, and wear-resistant, antifriction performance is also significantly improved; Nanometer MoS
2Interlayer can form the two-dimensional nano mixture after inserting organic group.
At present synthetic MoS
2Method high temperature solid-state method, presoma decomposition method, hydrogen reduction method, liquid phase reduction, chemical vapour deposition, vacuum laser sputter and electrolytic reaction etc. are arranged.But aforesaid method exists needs higher shortcomings such as synthesis temperature, working condition harshness, complex process and cost height, is unfavorable for scale operation and application.
[summary of the invention]
The objective of the invention is at above-mentioned existing problems, provide a kind of employing solvent-thermal method to prepare MoS
2The method of micron ball, this method reaction conditions gentleness, reaction process are simple, the productive rate height of product, purity height, favorable reproducibility.
Technical scheme of the present invention:
A kind of employing solvent-thermal method prepares MoS
2The method of micron ball, preparation process is as follows:
1) molybdenum source compound and sulphur source compound are mixed in the alcoholic solvent, fully stir and carry out supersound process it is fully disperseed; 2) finely dispersed mixture is transferred to carried out isothermal reaction in the reactor then; 3) MoS of black will can be made after reactant naturally cooling, separation, washing and the drying
2The micron ball.
Described molybdenum source compound is ammonium molybdate, Sodium orthomolybdate, potassium molybdate, ammonium paramolybdate, sodium paramolybdate, para-molybdic acid potassium or molybdic oxide.
Described sulphur source compound is thioacetamide, thiocarbamide, sulphur, ammonium sulfide, sodium sulphite, potassium sulphide, dithiocarbonic anhydride, Sulfothiorine, Potassium Thiosulphate or ammonium thiosulfate.
Described alcoholic solvent is ethanol, n-propyl alcohol, Virahol, propyl carbinol, ethylene glycol, 1,2-propylene glycol, 1, ammediol or glycerol.
The blending ratio of described molybdenum source compound and sulphur source compound is mol ratio 1: 1～15, and the blending ratio of molybdenum source compound and alcoholic solvent is that mass ratio is 1: 5～300.
The processing parameter of described supersound process is ultrasonic frequency 40kHz, supersound process time (1～30) minute.
The parameter of described isothermal reaction is temperature (100～240) ℃, reaction times (4～48) hour.
Described reactant washing methods is to use deionized water and absolute ethanol washing respectively 2～3 times, and drying temperature is 90 ℃.
Advantage of the present invention is the reaction conditions gentleness, the reaction favorable reproducibility, and preparation technology is simple, and preparation cost is low, and product yield and purity height are expected to produce in enormous quantities.The MoS of solvent thermal novel method preparation of the present invention
2Product all has very important application prospect at aspects such as energy storage, catalyzer and solid lubricants.
[description of drawings]
Fig. 1 is the prepared MoS of embodiment 1
2The XRD figure of micron ball.
Fig. 2 is the prepared MoS of embodiment 2
2The SEM figure of micron ball.
[embodiment]
Embodiment 1:
Taking by weighing 0.002mol Sodium orthomolybdate and 0.0045mol thiocarbamide is blended in the 50mL ethylene glycol, fully stirring and supersound process are 3 minutes, this mixture is transferred to autoclave, in 160 ℃ of following isothermal reactions 24 hours, naturally cooling then, use deionized water and absolute ethanol washing 2 times respectively, can obtain black MoS in 90 ℃ of following dryings
2The micron ball.
Fig. 1 is gained MoS
2The micron ball XRD figure, the reference standard card as can be seen, the synthetic material is the MoS of pure phase
2Crystalline material.
Embodiment 2:
Taking by weighing 0.005mol ammonium paramolybdate and 0.07mol thiocarbamide is blended in the 60mL glycerol, fully stirring and supersound process are 5 minutes, this mixture is transferred to autoclave, in 180 ℃ of following isothermal reactions 18 hours, naturally cooling then, use deionized water and absolute ethanol washing 3 times respectively, can obtain black MoS in 90 ℃ of following dryings
2The micron ball.
Fig. 2 is gained MoS
2The SEM figure of micron ball, as can be seen from the figure, the gained material is uniform micron ball, its granular size is approximately 1um.
Embodiment 3:
Taking by weighing 0.002mol ammonium molybdate and 0.002mol Sulfothiorine is blended in the 70mL n-propyl alcohol, fully stirring and supersound process are 5 minutes, this mixture is transferred to autoclave, in 190 ℃ of following isothermal reactions 12 hours, naturally cooling then, use deionized water and absolute ethanol washing 2 times respectively, can obtain black MoS in 90 ℃ of following dryings
2The micron ball.Detect demonstration, gained MoS through SEM figure
2Material is uniform micron ball.
Embodiment 4:
Take by weighing the 0.002mol molybdic oxide and the 0.002mol thioacetamide is blended in 80mL1, in the 2-propylene glycol, fully stirring and supersound process are 5 minutes, this mixture is transferred to autoclave, in 220 ℃ of following isothermal reactions 36 hours, naturally cooling is used deionized water and absolute ethanol washing 3 times respectively then, can obtain black MoS in 90 ℃ of following dryings
2The micron ball.Detect demonstration, gained MoS through SEM figure
2Material is uniform micron ball.
Claims (8)
1. one kind is adopted solvent-thermal method to prepare MoS
2The method of micron ball is characterized in that preparation process is as follows:
1) molybdenum source compound and sulphur source compound are mixed in the alcoholic solvent, fully stir and carry out supersound process it is fully disperseed; 2) finely dispersed mixture is transferred to carried out isothermal reaction in the reactor then; 3) MoS of black will can be made after reactant naturally cooling, separation, washing and the drying
2The micron ball.
2. prepare MoS according to the described employing solvent-thermal method of claim 1
2The method of micron ball, it is characterized in that: described molybdenum source compound is ammonium molybdate, Sodium orthomolybdate, potassium molybdate, ammonium paramolybdate, sodium paramolybdate, para-molybdic acid potassium or molybdic oxide.
3. prepare MoS according to the described employing solvent-thermal method of claim 1
2The method of micron ball, it is characterized in that: described sulphur source compound is thioacetamide, thiocarbamide, sulphur, ammonium sulfide, sodium sulphite, potassium sulphide, dithiocarbonic anhydride, Sulfothiorine, Potassium Thiosulphate or ammonium thiosulfate.
4. prepare MoS according to the described employing solvent-thermal method of claim 1
2The method of micron ball, it is characterized in that: described alcoholic solvent is ethanol, n-propyl alcohol, Virahol, propyl carbinol, ethylene glycol, 1,2-propylene glycol, 1, ammediol or glycerol.
5. prepare MoS according to the described employing solvent-thermal method of claim 1
2The method of micron ball, it is characterized in that: the blending ratio of described molybdenum source compound and sulphur source compound is mol ratio 1: 1～15, the blending ratio of molybdenum source compound and alcoholic solvent is that mass ratio is 1: 5～300.
6. prepare MoS according to the described employing solvent-thermal method of claim 1
2The method of micron ball, it is characterized in that: the processing parameter of described supersound process is ultrasonic frequency 40kHz, supersound process time (1～30) minute.
7. prepare MoS according to the described employing solvent-thermal method of claim 1
2The method of micron ball is characterized in that: the parameter of described isothermal reaction is temperature (100～240) ℃, reaction times (4～48) hour.
8. prepare MoS according to the described employing solvent-thermal method of claim 1
2The method of micron ball is characterized in that: described reactant washing methods is to use deionized water and absolute ethanol washing respectively 2～3 times, and drying temperature is 90 ℃.
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| CN102992281A (en) * | 2012-12-10 | 2013-03-27 | 江苏大学 | Nanometer flower-shaped MoSe2 and preparation method thereof |
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| CN104692464A (en) * | 2015-03-06 | 2015-06-10 | 济宁利特纳米技术有限责任公司 | Preparation of molybdenum disulfide quantum dots and application of molybdenum disulfide quantum dots in finished lubricant additive |
| CN104709892A (en) * | 2013-12-11 | 2015-06-17 | 中国科学院大连化学物理研究所 | Method for controllably preparing single layer and few layer molybdenum sulfide |
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| CN114832836A (en) * | 2022-05-16 | 2022-08-02 | 广西民族大学 | Micro-plastic catalyst, preparation method thereof and method for degrading micro-plastic |
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