CN110170294B - Monodisperse flower-like spherical MoS2Powder and preparation method thereof - Google Patents

Monodisperse flower-like spherical MoS2Powder and preparation method thereof Download PDF

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CN110170294B
CN110170294B CN201910444631.5A CN201910444631A CN110170294B CN 110170294 B CN110170294 B CN 110170294B CN 201910444631 A CN201910444631 A CN 201910444631A CN 110170294 B CN110170294 B CN 110170294B
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CN110170294A (en
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苏敏华
陈嘉威
徐作鹏
唐嘉枫
陈迪云
吴焰宏
张鸿郭
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Guangzhou University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/0262—Compounds of O, S, Se, Te
    • B01J20/0266—Compounds of S
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01J20/28019—Spherical, ellipsoidal or cylindrical
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    • C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract

The invention provides a monodisperse flower-like spherical MoS2The powder and the preparation method thereof comprise the following steps: uniformly dispersing molybdate and thiocyanate in an ionic liquid formed by imidazole type cations and halogen anions, uniformly mixing the dispersed molybdate and thiocyanate with a hydrochloric acid solution, and controlling the pH to be 1.7-1.1 to obtain a mixed system B; placing the mixed system B in a closed container, reacting for 24 hours at 220 ℃, and cooling to obtain a black product; washing the black product with water and an organic solvent, and drying to obtain monodisperse flower-like spherical MoS2And (3) powder. The method uses a hydrothermal method to prepare the monodisperse flower-ball-shaped MoS in one step2The ionic liquid is added into the raw materials and the pH value of the reaction system is controlled, so that the operation is simple and easy to control and the preparation conditions are easy to achieve; the preparation method is simple, the cost is low, and the monodisperse flower-like spherical MoS is obviously improved2The adsorption performance of (3). The flower-ball-shaped MoS prepared by the invention2The powder has large adsorption capacity and excellent adsorption performance.

Description

Monodisperse flower-like spherical MoS2Powder and preparation method thereof
Technical Field
The invention belongs to the field of preparation and application of inorganic functional materials, and particularly relates to monodisperse flower-like spherical MoS2Powder and a preparation method thereof.
Background
In the present day, dye contamination from different sources (such as textile industry, paper and pulp industry, dye industry, pharmaceutical industry, tanning industry and sulphate bleaching industry, etc.) has attracted a great deal of social attention. The treatment of organic dye pollution becomes an important task for environmental treatment. Molybdenum sulfide is used as a functional material and is found to have photocatalytic performance, but the existing preparation method of molybdenum sulfide has harsh conditions.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a monodisperse flower-ball-shaped MoS2Preparation method of powder, and preparation of monodisperse flower-ball-shaped MoS with excellent adsorption performance2And (3) powder.
In order to achieve the purpose, the invention adopts the technical scheme that: monodisperse flower-like spherical MoS2A method for preparing a powder, the method comprising the steps of:
(1) uniformly dispersing molybdate and thiocyanate in ionic liquid formed by imidazole type cations and halogen anions to obtain a mixed system A;
(2) uniformly mixing the mixed system A with a hydrochloric acid solution, and controlling the pH to be 1.7-1.1 to obtain a mixed system B;
(3) placing the mixed system B in a closed container, reacting for 24 hours at 220 ℃, and cooling to obtain a black product;
(4) washing the black product with water and an organic solvent, and drying to obtain monodisperse flower-like spherical MoS2And (3) powder.
The method uses a hydrothermal method to prepare the monodisperse flower-ball-shaped MoS in one step2The operation is simple and easy to control, and the preparation conditions are easy to reach; the preparation method is simple, the cost is low, and the monodisperse flower-like spherical MoS is obviously improved2The adsorption performance of (3).
Preferably, the ionic liquid is 1-butyl-3-methylimidazolium chloride.
Preferably, in the step (1), the dosage of the ionic liquid is as follows: 3mmol molybdate/mL ionic liquid.
Preferably, in the step (2), the mixed system A and the hydrochloric acid solution are uniformly mixed, and the pH is controlled to be 1.6-1.3, so as to obtain a mixed system B.
When the pH value of the mixed system B is controlled to be 1.6-1.3, the obtained monodisperse flower-ball-shaped MoS2The adsorption performance of the powder is better.
More preferably, in the step (2), the mixed system A and the hydrochloric acid solution are uniformly mixed, and the pH is controlled to be 1.4-1.3, so as to obtain a mixed system B.
Preferably, in the step (1), the molybdate is sodium molybdate, and the thiocyanate is sodium thiocyanate.
Preferably, in the step (1), the molybdate and the thiocyanate are used in the following amounts: the molar ratio of molybdenum element in molybdate to sulfur element in thiocyanate is 0.35: 1.
Preferably, in the step (3), the closed container is a high-pressure reaction kettle.
Preferably, in step (4), the organic solvent is ethanol.
Preferably, in the step (4), the drying temperature is 60 ℃ and the drying time is 12 h.
The invention also provides a monodisperse flower-ball-like MoS prepared by any one of the methods2And (3) powder.
The invention also provides the monodisperse flower-ball-shaped MoS2The powder is applied to removing organic pollutants in water as an adsorbent.
Monodisperse flower-like spherical MoS prepared by the invention2The powder has large adsorption capacity and excellent adsorption performance.
The invention has the beneficial effects that: the invention provides a monodisperse flower-like spherical MoS2The invention relates to powder and a preparation method thereof, and the method uses a hydrothermal method to prepare single-dispersed flower-ball-shaped MoS in one step2The ionic liquid is added into the raw materials and the pH value of the reaction system is controlled, so that the operation is simple and easy to control and the preparation conditions are easy to achieve; the preparation method is simple, the cost is low, and the monodisperse flower-like spherical MoS is obviously improved2The adsorption performance of (3). Monodisperse flower-like spherical MoS prepared by the invention2The powder has large adsorption capacity and excellent adsorption performance.
Drawings
FIG. 1 shows a monodisperse flower-ball-like MoS prepared according to an embodiment of the present invention2XRD pattern of the powder.
FIG. 2 shows a monodisperse flower-ball-like MoS prepared according to an embodiment of the present invention2Scanning Electron Microscope (SEM) morphology of the powder.
FIG. 3 shows a monodisperse flower-ball-like MoS prepared according to an embodiment of the present invention2Scanning Electron Microscope (SEM) morphology of the powder.
FIG. 4 shows a monodisperse flower-ball-like MoS prepared according to an embodiment of the present invention2The effect graph of the removal rate of the methyl orange absorbed by the powder in water.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to specific examples.
Example 1
Monodisperse flower-like spherical MoS as an example of the invention2A method for preparing a powder, the method comprising the steps of:
(1) weighing 0.72g of sodium molybdate dihydrate and 0.69g of sodium thiocyanate according to the molar ratio of Mo to S elements of 0.35:1, adding 1ml of 1-butyl-3-methylimidazolium chloride ionic liquid into a beaker, stirring to dissolve the two kinds of powder, and uniformly mixing to obtain a mixed system A;
(2) taking 0.6ml of concentrated hydrochloric acid, adding the concentrated hydrochloric acid into 60ml of deionized water, stirring and mixing, mixing a hydrochloric acid solution with the mixed system A, and magnetically stirring for 15 minutes until the pH value of the solution is 1.7 to obtain a mixed system B;
(3) transferring the mixed system B into a 100ml reaction kettle, sealing, transferring into a high-temperature reaction box, setting the reaction temperature at 220 ℃, setting the reaction time at 24 hours, and cooling to room temperature after the reaction is finished to obtain a black product;
(4) and (3) respectively centrifugally washing the black product by using deionized water and absolute ethyl alcohol for 3 times, wherein the rotating speed of a centrifugal machine is 5000 revolutions per minute, the centrifugal time is 5 minutes, drying the obtained centrifugal product in a vacuum drying oven at 60 ℃ for 12 hours, and cooling to room temperature to obtain the monodisperse flower-ball-like MoS2And (3) powder.
Example 2
Monodisperse flower-like spherical MoS as an example of the invention2A method for preparing a powder, the method comprising the steps of:
(1) weighing 0.72g of sodium molybdate dihydrate and 0.69g of sodium thiocyanate according to the molar ratio of Mo to S elements of 0.35:1, adding 1ml of 1-butyl-3-methylimidazolium chloride ionic liquid into a beaker, stirring to dissolve the two kinds of powder, and uniformly mixing to obtain a mixed system A;
(2) taking 0.7ml of concentrated hydrochloric acid, adding the concentrated hydrochloric acid into 60ml of deionized water, stirring and mixing, mixing a hydrochloric acid solution with the mixed system A, and magnetically stirring for 15 minutes until the pH value of the solution is 1.6 to obtain a mixed system B;
(3) transferring the mixed system B into a 100ml reaction kettle, sealing, transferring into a high-temperature reaction box, setting the reaction temperature at 220 ℃, setting the reaction time at 24 hours, and cooling to room temperature after the reaction is finished to obtain a black product;
(4) centrifuging and washing the black product for 3 times by using deionized water and absolute ethyl alcohol respectively, wherein the rotating speed of a centrifuge is 5000 r/min, the centrifuging time is 5 minutes, drying the obtained centrifugal product in a vacuum drying oven at 60 ℃ for 12 hours, and cooling to room temperature to obtain the monodisperseFlower-like spherical MoS2And (3) powder.
Example 3
Monodisperse flower-like spherical MoS as an example of the invention2A method for preparing a powder, the method comprising the steps of:
(1) weighing 0.72g of sodium molybdate dihydrate and 0.69g of sodium thiocyanate according to the molar ratio of Mo to S elements of 0.35:1, adding 1ml of 1-butyl-3-methylimidazolium chloride ionic liquid into a beaker, stirring to dissolve the two kinds of powder, and uniformly mixing to obtain a mixed system A;
(2) taking 0.8ml of concentrated hydrochloric acid, adding the concentrated hydrochloric acid into 60ml of deionized water, stirring and mixing, mixing a hydrochloric acid solution with the mixed system A, and magnetically stirring for 15 minutes until the pH value of the solution is 1.5 to obtain a mixed system B;
(3) transferring the mixed system B into a 100ml reaction kettle, sealing, transferring into a high-temperature reaction box, setting the reaction temperature at 220 ℃, setting the reaction time at 24 hours, and cooling to room temperature after the reaction is finished to obtain a black product;
(4) and (3) respectively centrifugally washing the black product by using deionized water and absolute ethyl alcohol for 3 times, wherein the rotating speed of a centrifugal machine is 5000 revolutions per minute, the centrifugal time is 5 minutes, drying the obtained centrifugal product in a vacuum drying oven at 60 ℃ for 12 hours, and cooling to room temperature to obtain the monodisperse flower-ball-like MoS2And (3) powder.
Example 4
Monodisperse flower-like spherical MoS as an example of the invention2A method for preparing a powder, the method comprising the steps of:
(1) weighing 0.72g of sodium molybdate dihydrate and 0.69g of sodium thiocyanate according to the molar ratio of Mo to S elements of 0.35:1, adding 1ml of 1-butyl-3-methylimidazolium chloride ionic liquid into a beaker, stirring to dissolve the two kinds of powder, and uniformly mixing to obtain a mixed system A;
(2) taking 0.9ml of concentrated hydrochloric acid, adding the concentrated hydrochloric acid into 60ml of deionized water, stirring and mixing, mixing a hydrochloric acid solution with the mixed system A, and magnetically stirring for 15 minutes until the pH value of the solution is 1.4 to obtain a mixed system B;
(3) transferring the mixed system B into a 100ml reaction kettle, sealing, transferring into a high-temperature reaction box, setting the reaction temperature at 220 ℃, setting the reaction time at 24 hours, and cooling to room temperature after the reaction is finished to obtain a black product;
(4) and (3) respectively centrifugally washing the black product by using deionized water and absolute ethyl alcohol for 3 times, wherein the rotating speed of a centrifugal machine is 5000 revolutions per minute, the centrifugal time is 5 minutes, drying the obtained centrifugal product in a vacuum drying oven at 60 ℃ for 12 hours, and cooling to room temperature to obtain the monodisperse flower-ball-like MoS2And (3) powder.
Example 5
Monodisperse flower-like spherical MoS as an example of the invention2A method for preparing a powder, the method comprising the steps of:
(1) weighing 0.72g of sodium molybdate dihydrate and 0.69g of sodium thiocyanate according to the molar ratio of Mo to S elements of 0.35:1, adding 1ml of 1-butyl-3-methylimidazolium chloride ionic liquid into a beaker, stirring to dissolve the two kinds of powder, and uniformly mixing to obtain a mixed system A;
(2) taking 1.0ml of concentrated hydrochloric acid, adding the concentrated hydrochloric acid into 60ml of deionized water, stirring and mixing, mixing a hydrochloric acid solution with the mixed system A, and magnetically stirring for 15 minutes until the pH value of the solution is 1.3 to obtain a mixed system B;
(3) transferring the mixed system B into a 100ml reaction kettle, sealing, transferring into a high-temperature reaction box, setting the reaction temperature at 220 ℃, setting the reaction time at 24 hours, and cooling to room temperature after the reaction is finished to obtain a black product;
(4) and (3) respectively centrifugally washing the black product by using deionized water and absolute ethyl alcohol for 3 times, wherein the rotating speed of a centrifugal machine is 5000 revolutions per minute, the centrifugal time is 5 minutes, drying the obtained centrifugal product in a vacuum drying oven at 60 ℃ for 12 hours, and cooling to room temperature to obtain the monodisperse flower-ball-like MoS2And (3) powder.
Example 6
Monodisperse flower-like spherical MoS as an example of the invention2A method for preparing a powder, the method comprising the steps of:
(1) weighing 0.72g of sodium molybdate dihydrate and 0.69g of sodium thiocyanate according to the molar ratio of Mo to S elements of 0.35:1, adding 1ml of 1-butyl-3-methylimidazolium chloride ionic liquid into a beaker, stirring to dissolve the two kinds of powder, and uniformly mixing to obtain a mixed system A;
(2) taking 1.1ml of concentrated hydrochloric acid, adding the concentrated hydrochloric acid into 60ml of deionized water, stirring and mixing, mixing a hydrochloric acid solution with the mixed system A, and magnetically stirring for 15 minutes until the pH value of the solution is 1.3 to obtain a mixed system B;
(3) transferring the mixed system B into a 100ml reaction kettle, sealing, transferring into a high-temperature reaction box, setting the reaction temperature at 220 ℃, setting the reaction time at 24 hours, and cooling to room temperature after the reaction is finished to obtain a black product;
(4) and (3) respectively centrifugally washing the black product by using deionized water and absolute ethyl alcohol for 3 times, wherein the rotating speed of a centrifugal machine is 5000 revolutions per minute, the centrifugal time is 5 minutes, drying the obtained centrifugal product in a vacuum drying oven at 60 ℃ for 12 hours, and cooling to room temperature to obtain the monodisperse flower-ball-like MoS2And (3) powder.
Example 7
Monodisperse flower-like spherical MoS as an example of the invention2A method for preparing a powder, the method comprising the steps of:
(1) weighing 0.72g of sodium molybdate dihydrate and 0.69g of sodium thiocyanate according to the molar ratio of Mo to S elements of 0.35:1, adding 1ml of 1-butyl-3-methylimidazolium chloride ionic liquid into a beaker, stirring to dissolve the two kinds of powder, and uniformly mixing to obtain a mixed system A;
(2) taking 1.2ml of concentrated hydrochloric acid, adding the concentrated hydrochloric acid into 60ml of deionized water, stirring and mixing, mixing a hydrochloric acid solution with the mixed system A, and magnetically stirring for 15 minutes until the pH value of the solution is 1.2 to obtain a mixed system B;
(3) transferring the mixed system B into a 100ml reaction kettle, sealing, transferring into a high-temperature reaction box, setting the reaction temperature at 220 ℃, setting the reaction time at 24 hours, and cooling to room temperature after the reaction is finished to obtain a black product;
(4) and (3) respectively centrifugally washing the black product by using deionized water and absolute ethyl alcohol for 3 times, wherein the rotating speed of a centrifugal machine is 5000 revolutions per minute, the centrifugal time is 5 minutes, drying the obtained centrifugal product in a vacuum drying oven at 60 ℃ for 12 hours, and cooling to room temperature to obtain the monodisperse flower-ball-like MoS2And (3) powder.
Example 8
As one example of the inventionMonodisperse flower-like spherical MoS2A method for preparing a powder, the method comprising the steps of:
(1) weighing 0.72g of sodium molybdate dihydrate and 0.69g of sodium thiocyanate according to the molar ratio of Mo to S elements of 0.35:1, adding 1ml of 1-butyl-3-methylimidazolium chloride ionic liquid into a beaker, stirring to dissolve the two kinds of powder, and uniformly mixing to obtain a mixed system A;
(2) taking 1.3ml of concentrated hydrochloric acid, adding the concentrated hydrochloric acid into 60ml of deionized water, stirring and mixing, mixing a hydrochloric acid solution with the mixed system A, and magnetically stirring for 15 minutes until the pH value of the solution is 1.2 to obtain a mixed system B;
(3) transferring the mixed system B into a 100ml reaction kettle, sealing, transferring into a high-temperature reaction box, setting the reaction temperature at 220 ℃, setting the reaction time at 24 hours, and cooling to room temperature after the reaction is finished to obtain a black product;
(4) and (3) respectively centrifugally washing the black product by using deionized water and absolute ethyl alcohol for 3 times, wherein the rotating speed of a centrifugal machine is 5000 revolutions per minute, the centrifugal time is 5 minutes, drying the obtained centrifugal product in a vacuum drying oven at 60 ℃ for 12 hours, and cooling to room temperature to obtain the monodisperse flower-ball-like MoS2And (3) powder.
Example 9
Monodisperse flower-like spherical MoS as an example of the invention2A method for preparing a powder, the method comprising the steps of:
(1) weighing 0.72g of sodium molybdate dihydrate and 0.69g of sodium thiocyanate according to the molar ratio of Mo to S elements of 0.35:1, adding 1ml of 1-butyl-3-methylimidazolium chloride ionic liquid into a beaker, stirring to dissolve the two kinds of powder, and uniformly mixing to obtain a mixed system A;
(2) taking 1.4ml of concentrated hydrochloric acid, adding the concentrated hydrochloric acid into 60ml of deionized water, stirring and mixing, mixing a hydrochloric acid solution with the mixed system A, and magnetically stirring for 15 minutes until the pH value of the solution is 1.1 to obtain a mixed system B;
(3) transferring the mixed system B into a 100ml reaction kettle, sealing, transferring into a high-temperature reaction box, setting the reaction temperature at 220 ℃, setting the reaction time at 24 hours, and cooling to room temperature after the reaction is finished to obtain a black product;
(4) the black products were respectively deionizedWater and absolute ethyl alcohol are centrifugally washed for 3 times, the rotating speed of a centrifugal machine is 5000 r/min, the centrifugal time is 5 minutes, the obtained centrifugal product is dried for 12 hours in a vacuum drying box at the temperature of 60 ℃, and the monodisperse flower-ball-shaped MoS is obtained after the product is cooled to the room temperature2And (3) powder.
Experimental example 1
For the monodisperse flower-ball-like MoS prepared by the embodiment of the invention2And carrying out scanning electron microscope test and X-ray diffraction test on the powder.
The method parameters are as follows:
the field emission scanning electron microscope equipment is a field emission scanning electron microscope (JSM-7001F), and the main specifications and technical indexes are as follows:
1. resolution is 1.2nm (30kV) and 3.0nm (1 kV);
2. acceleration voltage: 0.5kV to 30 kV;
3. magnification: 25 times to 100 ten thousand times;
4. an electron gun: an immersed thermal field emission electron gun with a maximum current of 200 nA; a detector: a secondary electron detector; beam current range: 10-12-2X 10-7A; an objective lens: pole shoe of the non-magnetic leakage objective lens;
5. a sample chamber: the maximum loadable sample diameter is 200 mm;
6. the INCA electric refrigeration energy spectrometer system is equipped, and the energy spectrum detection range is as follows: be 4-U92.
Secondly, the X-ray diffraction equipment is a (PW3040/60) type X-ray powder diffractometer, and the X-ray source is a Cu target.
From FIG. 1, it can be seen that all diffraction peaks in the graph are MoS with hexagonal structure2And no other hetero-phase components.
Experimental example 2
Test examples 1-9 monodisperse variegated-ball-like MoS2The powder has the adsorption performance on methyl orange in water.
Adding monodisperse flower ball-like MoS into methyl orange organic dye water with concentration of 20mg/L2The powder is mixed evenly, and the dosage is 0.5 g/L.
The concentration of methyl orange in water was tested at 5 minutes; and a model UV-2550 spectrophotometer at 463nm wavelength to analyze the residual dye concentration.
FIG. 3 is a histogram of the removal rate, from which it can be seen that the monodisperse flower-ball-like MoS of examples 1 to 92The powder has beneficial adsorption performance on methyl orange in water, the adsorption time is 5 minutes, and the adsorption removal rate is over 60 percent; and monodisperse flower-like spherical MoS when pH is controlled to 1.6-1.32The powder has better adsorption performance, wherein the adsorption performance of example 4 is the most excellent.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.

Claims (4)

1. Monodisperse flower-like spherical MoS with hexagonal structure2The preparation method of the powder is characterized by comprising the following steps:
(1) uniformly dispersing molybdate and thiocyanate in ionic liquid formed by imidazole type cations and halogen anions to obtain a mixed system A; the molybdate is sodium molybdate, and the thiocyanate is sodium thiocyanate; the ionic liquid is 1-butyl-3-methylimidazole chloride salt, and the dosage of the ionic liquid is as follows: 3mmol of molybdate/mL of ionic liquid, wherein the molar ratio of molybdenum element in the sodium molybdate to sulfur element in the sodium thiocyanate is 0.35: 1;
(2) uniformly mixing the mixed system A with a hydrochloric acid solution, and controlling the pH to be 1.6-1.3 to obtain a mixed system B;
(3) placing the mixed system B in a closed container, reacting for 24 hours at 220 ℃, and cooling to obtain a black product;
(4) washing the black product with water and an organic solvent, and drying to obtain monodisperse flower-like spherical MoS2And the organic solvent is ethanol.
2. The method according to claim 1, wherein in the step (4), the drying temperature is 60 ℃ and the drying time is 12 h.
3. Monodisperse flower-ball-like MoS with hexagonal structure prepared by the method according to any of claims 1-22And (3) powder.
4. Monodisperse flower-ball-like MoS with hexagonal structure according to claim 32The powder is applied to removing organic pollutants in water as an adsorbent.
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CN1994895A (en) * 2006-12-20 2007-07-11 浙江大学 Preparation method for ion liquid assisted hydrothermal synthesis of MoS2 microsphere
CN105435818A (en) * 2014-09-25 2016-03-30 中国科学院大连化学物理研究所 Surface amphiphilic nano-molybdenum disulfide hydrogenation catalyst and preparation method and application thereof
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Hao Luo, et al.Hydrothermal synthesis of hollow MoS2 microspheres in ionic liquids/water binary emulsions.《Materials Letters》.2008,第62卷第3558页右栏第3段至第3559页左栏第1段及图2. *
Hydrothermal synthesis of hollow MoS2 microspheres in ionic liquids/water binary emulsions;Hao Luo, et al;《Materials Letters》;20080328;第62卷;第3558页右栏第3段至第3559页左栏第1段及图2 *
Ionic liquid assisted hydrothermal synthesis of hollow core/shell MoS2 microspheres;Jiahe Li;《Materials Letters》;20150810;第160卷;第550页右栏第3段至第551页左栏第1段 *
Synthesis of bilayer MoS2 nanosheets by a facile hydrothermal method and their methyl orange adsorption capacity;Lijuan Ye, et al;《Materials Research Bulletin》;20140419;第55卷;第222页左栏第2段至右栏第1段及摘要部分 *

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