CN105417581A - Method for complexing hydrothermal synthesis of uniform flower-like MoS2 nanospheres - Google Patents

Method for complexing hydrothermal synthesis of uniform flower-like MoS2 nanospheres Download PDF

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CN105417581A
CN105417581A CN201410436988.6A CN201410436988A CN105417581A CN 105417581 A CN105417581 A CN 105417581A CN 201410436988 A CN201410436988 A CN 201410436988A CN 105417581 A CN105417581 A CN 105417581A
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mos
complexing
homogeneous
hydrothermal synthesis
bouquet
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田志坚
李佳鹤
王冬娥
姜玉霞
李敏
马怀军
潘振栋
曲炜
李鹏
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Dalian Institute of Chemical Physics of CAS
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Dalian Institute of Chemical Physics of CAS
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Abstract

The present invention discloses a method for complexing hydrothermal synthesis of uniform flower-like MoS2 nanospheres. The method comprises: sequentially dissolving a certain amount of a molybdenum source, a sulfur source and a complexing agent in deionized water to form a solution, regulating the molybdenum source concentration to 0.04-0.16 M, regulating a molar ratio of the sulfur source to the molybdenum source to 2:7-4:1, and regulating a molar ratio of the complexing agent to the molybdenum source to 2-6; placing the prepared solution in a closed hydrothermal reaction kettle, controlling the reaction temperature at 120-200 DEG C, and controlling the reaction time at 24-72 h; and after completing the reaction, cooling, carrying out suction filtration, washing, and drying to obtain the flower-like MoS2 nanospheres. According to the present invention, the synthesis method has advantages of mild condition, simple operation, uniform product morphology and particle size, good product dispersion property, and high yield; and the synthesized flower-like MoS2 nanospheres adopted as oil product hydrogenation catalysts, electrode materials, solid lubricants and the like have wide applications.

Description

The homogeneous MoS of a kind of complexing Hydrothermal Synthesis 2the method of nanometer bouquet
Technical field
The invention belongs to inorganic nano material synthesis field, be specifically related to the homogeneous MoS of a kind of complexing Hydrothermal Synthesis 2the method of nanometer bouquet.
Background technology
MoS 2be the main component of molybdenum glance, in its crystalline structure, there is a kind of sandwich flaggy: two-layer S atom therebetween one deck Mo atom, form " sandwich " sandwich structure.In layer, atom is with strong covalent bonds, and interlayer is then more weak Van der Waals force, is easy between layers peel off, and has good anisotropy and lower rubbing factor.MoS 2in crystal each molybdenum atom surround by six sulphur atoms, in triangular prism column, expose a lot of Mo-S faceted pebble, can be used as catalytic active center.The nano intercalation compounding material formed after other groups of Intercalation reaction has the physicals of many excellences.In addition, molybdenumdisulphide is a kind of diamagnetism and has the compound of semiconductor property, has good optical, electrical, lubrication and catalytic performance.
Nanometer MoS 2with the MoS of common size 2compare, its antifriction quality, resistance to abrasion, fuel economy and extreme pressure property all improve a lot.Because the atom of nanoparticle or molecule are in metastable state in a large number, be thermodynamically unstable, its surface atom periphery lacks adjacent atom, has a lot of dangling bonds, is easily combined with other atoms, therefore has very high chemically reactive.Nano level MoS 2particle specific surface is large, and high adsorption capacity, reactive behavior is high, and its catalytic performance especially catalytic desulfurhydrogenation performance is very strong.
At present, MoS 2synthetic method is broadly divided into three major types: high-temperature gas-solid phase synthesi, physics synthetic method and wet chemistry synthesis method.Y.Feldman etc. (267 volumes, the 222nd page) on nineteen ninety-five Science periodical have delivered a kind of method, use diamond heating MoO 3to about 850 DEG C, pass to H 2s+ (H 2+ N 2) reducing gas, MoO in high-temperature reductibility atmosphere 3and H 2s gas reaction, preparation synthesis MoS 2fullerene nanoparticle and nanotube.Chinese patent CN102616854A discloses a kind of monodisperse spherical MoS 2the preparation method of superfine powder, first obtained MoS 3, then 500-800 DEG C of reduction in hydrogen.Chinese patent CN1837064 discloses and a kind of adopts molybdate and sulphur is high temperature vulcanized prepares MoS 2method.Chinese patent CN101224905 disclose a kind of with elemental sulfur and molybdic oxide for raw material, being carrier gas with argon gas, is that reducing gas synthesizes spherical MoS with hydrogen 2method.US Patent No. 4243553A1 discloses a kind of MoS preparing high-ratio surface 2method, adopt Thiomolybdate 300-800 DEG C of high-temperature calcination preparation under an inert atmosphere.Gas-solid method preparation condition is harsh, higher to the requirement of facility environment, and needs to use toxic gas H 2s etc., the product of gained not easily disperses.Physical is to MoS by the means such as mechanical mill, high energy physics 2carry out pulverizing, cut or spraying thus reach refinement or obtain the object of coating.Zhou Lichun etc. (23 volumes, 6 phases, 618-621 page) on electron microscopic journal in 2004 have delivered one section of paper, adopt supersonic jet mill to pulverize molybdenumdisulphide powder, thus obtain nano molybdenum disulfide.The requirement of this method to equipment is higher, and products obtained therefrom kind is less, and the size of nanoparticle is difficult to be controlled, and method is dumb, and thus its application is very limited.
Wet chemistry synthesis method mild condition, simple to operate, be a kind of advantageous synthetic method.Chinese patent CN1468945 discloses that one adds oleic acid in the solution, stearic acid is that coating materials prepares oil-dispersing property MoS 2method.Chinese patent CN102142551A discloses a kind of method of a step Hydrothermal Synthesis graphene nanometer sheet/molybdenumdisulphide composite nano materials.But the nanosized product of Hydrothermal Synthesis is often easily reunited, size and pattern are difficult to regulation and control.Chinese patent CN101113021 discloses a kind of interpolation inorganic additives Tungstenic compound or titanium-containing compound hydro-thermal prepares flower-shaped MoS 2the method of microballoon.Chinese patent CN1994895A discloses a kind of ionic liquid assisted hydrothermal synthesis MoS 2the preparation method of microballoon, Chinese patent CN101851006A discloses a kind of solvent-thermal method and prepares MoS 2the method of microballoon, Chinese patent CN102938461A discloses a kind of MoS of nanometer sheet self-assembly 2the preparation method of nano-hollow material, all obtains comparatively homogeneous product.But because ionic liquid etc. is generally macromole, it forms MoS after self-assembly in aqueous 2the template of growth, prepared Product size is comparatively large, and how in micron level, specific surface is less, and activity is lower.
Summary of the invention
The object of the invention is for above-mentioned existing problems, provide one to utilize the homogeneous MoS of complexing Hydrothermal Synthesis 2the method of nanometer bouquet.
The method applied in the present invention is as follows:
1. obtain solution: molybdenum source, sulphur source, complexing agent are successively dissolved in deionized water and form homogeneous solution.
2. hydro-thermal reaction: be transferred to by solution in hydrothermal reaction kettle, sealing, is placed in baking oven 120 ~ 200 DEG C of hydro-thermal reactions 24 ~ 72 hours.
3. separating, washing: adopt conventional separation means, as suction filtration, precipitate with deionized water and absolute ethanol washing, dry, obtain black powder sample.
4. phenetic analysis: products therefrom XRD (X-ray powder diffraction) carries out degree of crystallinity sign to it, result display gained black powder is MoS 2, degree of crystallization is good; Its pattern is characterized, the MoS of SEM photo (see Fig. 2, Fig. 3) display preparation with SEM (scanning electronic microscope) 2for the nanometer bouquet of particle diameter between 200 ~ 500nm (a kind of lamella accumulation, shaggy ball-like structure), pattern, size uniformity, favorable dispersity.
The above molybdenum source is the molybdate Sodium orthomolybdate of solubility or ammonium molybdate or the mixture of the two, and sulphur source used is easily molten and sodium sulphite in alkalescence or potassium sulphide or ammonium sulfide or its mixture, and complexing agent used is carboxylic oxalic acid or citric acid.The concentration in molybdenum source is 0.04 ~ 0.16M; Sulphur source is 2:7 ~ 4:1 with the ratio of the amount of substance in molybdenum source; Complexing agent is 2 ~ 6:1 with the ratio of the amount of substance in molybdenum source.
In reaction process, the carboxyl in complexing agent molecule can form complex compound with molybdate ion coordination.Containing multiple carboxyl in each complexing agent molecule, different with concentration according to the valence state of molybdenum acid ion, these carboxyls can while coordination molybdate ion, also can distinguish two or three molybdate ions of coordination.For citric acid complex ammonium molybdate: each Mo 7o 24 6-can with six carboxyl coordinations, if the coordination simultaneously of three carboxyls in each citric acid molecule molybdenum acid ion, then a molybdenum acid ion and two citric acid molecule form complexing body; If coordination three molybdate ions respectively of three carboxyls in citric acid, then a molybdenum acid ion needs and six citric acid molecule complexings, forms the large complexing body of many metal centers.Therefore pass through the proportioning in modulation complexing agent and molybdenum source, the size of complex compound can be controlled, thus control the size of final product.Due to the complexing of complexing agent and molybdate, molybdate ion concentration free in environment is inevitable lower, and the sulphur source added with molybdate-complexing agent complexes body, reduction-sulfurization effect slowly can occur, the sulfide M oS of formation 2orderly nano flower spherical structure can be assembled into according to the array mode of molybdate presoma in complex compound.This process is slower than the raw material Direct Hydrothermal speed of response of routine, is similar to precipitation from homogeneous solution process, is conducive to obtaining the product that size, pattern are homogeneous.Reaction equation following (with ammonium molybdate and sodium sulphite for raw material, citric acid is the reaction of complexing agent is example):
9(NH 4) 2MoO 4+18Na 2S+C 6H 8O 7·H 2O+4H 2O→9MoS 2+36NaOH+6CO 2+18NH 3
The present invention compared with prior art tool has the following advantages and effect:
Hydrothermal temperature of the present invention is 120 ~ 200 DEG C, and the time is 24 ~ 72 hours, and condition is comparatively gentle.Complexing agent citric acid of the present invention and oxalic acid are the reductive agents of reaction simultaneously, avoid the reductive agent using the danger such as hydrazine hydrate, and decrease the introduction volume of impurity.
The invention provides a kind of method of effective control hydrothermal product pattern, size, homogeneity, namely form complex compound by interpolation complexing agent and molybdate ion, on the one hand sequential reduction sulfidation is slowly carried out, generate homogeneous, few product of reuniting; Make the MoS produced on the other hand 2regular nanometer flower structure can be become by ordered fabrication.By regulating material concentration and the proportioning with complexing agent thereof, the size of Complexes In Solution can be changed, thus change the size of final product.The method can be used for the Morphological control of analogous material.
Product prepared by the present invention is the homogeneous MoS of particle diameter 200-500nm 2nanometer bouquet, its pattern and size uniformity, good dispersity.Compared with the hydrothermal product of routine, the method applied in the present invention both effectively reduced reunion, and size remains on Nano grade again.MoS prepared by the present invention 2nanometer bouquet is formed by lamella accumulation, surface irregularity, and the avtive spot of exposure is many, and adsorptive power and permeability are very strong, and reactive behavior is higher.In addition, product is easy to separate from solution, adopts conventional suction filtration means, gained MoS 2more than 95% of the yield accessibility theory yield of product.
The MoS of the present invention's synthesis 2nanometer bouquet tool in oil hydrogenation catalysis, electrochemical electrode material and solid lubrication etc. has been widely used.Especially, product morphology is homogeneous, size is less, is expected to in battery, sensor sophisticated equipment.
Accompanying drawing explanation
Fig. 1 is the MoS that when not adding complexing agent prepared by hydro-thermal 2sEM figure, in contrast;
Fig. 2 is embodiment 4 MoS that prepared by hydro-thermal when adding citric acid complex 2sEM figure (raw material ammonium molybdate concentration is 0.04M) of nanometer bouquet;
Fig. 3 is embodiment 5 MoS that prepared by hydro-thermal when adding citric acid complex 2sEM figure (raw material ammonium molybdate concentration is 0.05M) of nanometer bouquet;
Fig. 4 is embodiment 4 MoS that prepared by hydro-thermal when adding citric acid complex 2the XRD figure (raw material ammonium molybdate concentration is 0.04M) of nanometer bouquet, what mark in figure is respectively MoS 2002,100 and 110 peaks.
Embodiment
Below in conjunction with specific experiment example, the present invention is described in further detail.
Embodiment 1:
The Sodium orthomolybdate of 5mmol is dissolved in 50ml deionized water, forms the solution of 0.1M, add the potassium sulphide of 20mmol, stir.Then the oxalic acid of 12mmol is added.After abundant stirring, this solution is transferred in 100ml water heating kettle, with 120 DEG C at react 24 hours, naturally cool to room temperature, suction filtration, precipitate with deionized water and absolute ethanol washing, 70 DEG C of dried in vacuo overnight, collect MoS 2sample.Carry out SEM sign to sample, SEM result display products therefrom is the nanometer bouquet of particle diameter about 200nm, and bouquet is piled up by a large amount of laminated structure and formed, better dispersed.
Embodiment 2:
The Sodium orthomolybdate of 3.5mmol is dissolved in 50ml deionized water, forms the solution of 0.07M, add the ammonium sulfide of 12mmol, stir.Then the oxalic acid of 8.3mmol is added.After abundant stirring, this solution is transferred in 100ml water heating kettle, reacts 36 hours at 140 DEG C, naturally cool to room temperature, suction filtration, precipitate with deionized water and absolute ethanol washing, 70 DEG C of dried in vacuo overnight, collect MoS 2sample.Carry out SEM sign to sample, SEM result display products therefrom is the nanometer bouquet of particle diameter about 300nm, and bouquet is piled up by laminated structure and formed, better dispersed.
Embodiment 3:
The ammonium molybdate of 2.5mmol is dissolved in 50ml deionized water, forms the solution of 0.05M, add the ammonium sulfide of 10mmol, stir.Then the oxalic acid of 7.5mmol is added.After abundant stirring, this solution is transferred in 100ml water heating kettle, with 160 DEG C at react 48 hours, naturally cool to room temperature, suction filtration, precipitate with deionized water and absolute ethanol washing, 70 DEG C of dried in vacuo overnight, collect MoS 2sample.Carry out SEM sign to sample, SEM result display products therefrom is the nanometer bouquet of particle diameter about 200-300nm, and bouquet is piled up by laminated structure and formed, better dispersed.
Embodiment 4:
The ammonium molybdate of 2mmol is dissolved in 50ml deionized water, forms the solution of 0.04M, add the sodium sulphite of 8mmol, stir.Then the citric acid of 4.8mmol is added.After abundant stirring, this solution is transferred in 100ml water heating kettle, with 180 DEG C at react 48 hours, naturally cool to room temperature, suction filtration, precipitate with deionized water and absolute ethanol washing, 70 DEG C of dried in vacuo overnight, collect MoS 2sample.As a comparison, do not add citric acid, the identical Hydrothermal Synthesis MoS of other conditions 2sample.Carry out XRD and SEM to two kinds of samples to characterize, find that two kinds of product components are MoS 2but the product adding citric acid complex is the nanometer bouquet of particle diameter about 400nm, bouquet is piled up by laminated structure and is formed, favorable dispersity, and does not add laminated structure uneven sized by the sample of citric acid, and reunite serious (see Fig. 1 and Fig. 2).
Embodiment 5:
The ammonium molybdate of 2.5mmol is dissolved in 50ml deionized water, forms the solution of 0.05M, add the sodium sulphite of 10mmol, stir.Then the citric acid of 5mmol is added.After abundant stirring, this solution is transferred in 100ml water heating kettle, with 180 DEG C at react 48 hours, naturally cool to room temperature, suction filtration, precipitate with deionized water and absolute ethanol washing, 70 DEG C of dried in vacuo overnight, collect MoS 2sample.Carry out SEM sign to sample, SEM result display products therefrom is the class ball shaped nano bouquet structure of particle diameter 200-300nm, and bouquet is piled up by laminated structure and formed, favorable dispersity.(see Fig. 3)
Embodiment 6:
The ammonium molybdate of 2.5mmol is dissolved in 50ml deionized water, forms the solution of 0.05M, add the sodium sulphite of 10mmol, stir.Then the citric acid of 7.5mmol is added.After abundant stirring, this solution is transferred in 100ml water heating kettle, reacts 72 hours at 200 DEG C, naturally cool to room temperature, suction filtration, precipitate with deionized water and absolute ethanol washing, 70 DEG C of dried in vacuo overnight, collect MoS 2sample.Carry out SEM sign to sample, SEM result display products therefrom is the nanometer bouquet of particle diameter about 200-300nm, and bouquet is piled up by laminated structure and formed, better dispersed.

Claims (9)

1. the homogeneous MoS of complexing Hydrothermal Synthesis 2the method of nanometer bouquet, it is characterized in that comprising the following steps: molybdenum source, sulphur source, complexing agent are dissolved in deionized water and form solution, join solution and be placed in airtight hydrothermal reaction kettle, heat up and carry out hydro-thermal reaction, reaction terminates rear separate solid product, obtains MoS 2nanometer bouquet.
2. the homogeneous MoS of complexing Hydrothermal Synthesis according to claim 1 2the method of nanometer bouquet, is characterized in that: molybdenum source used is the ammonium molybdate of solubility or Sodium orthomolybdate or the mixture of the two.
3. the homogeneous MoS of complexing Hydrothermal Synthesis according to claim 1 2the method of nanometer bouquet, is characterized in that: sulphur source used is a kind of or mixture of any two in the sodium sulphite of solubility, potassium sulphide or ammonium sulfide or the mixture of three.
4. the homogeneous MoS of complexing Hydrothermal Synthesis according to claim 1 2the method of nanometer bouquet, is characterized in that: complexing agent used is one in oxalic acid or citric acid or two kinds.
5. the homogeneous MoS of complexing Hydrothermal Synthesis according to claim 1 2the method of nanometer bouquet, is characterized in that: material is followed successively by molybdenum source, sulphur source and complexing agent to order of addition in deionized water.
6. the homogeneous MoS of complexing Hydrothermal Synthesis according to claim 1 2the method of nanometer bouquet, is characterized in that: the preparation method of employing is low-temperature hydrothermal reaction, and temperature is 120 ~ 200 DEG C.
7. the homogeneous MoS of complexing Hydrothermal Synthesis according to claim 1 2the method of nanometer bouquet, is characterized in that: the hydro-thermal reaction time is 24 ~ 72 hours.
8. the homogeneous MoS of complexing Hydrothermal Synthesis according to claim 1 2the method of nanometer bouquet, is characterized in that: in raw material, the concentration in molybdenum source controls between 0.04-0.16M;
Sulphur source controls at 2:7 ~ 4:1 with the ratio of the amount of substance in molybdenum source;
Complexing agent is 2 ~ 6:1 with the ratio of the amount of substance in molybdenum source.
9. the homogeneous MoS of complexing Hydrothermal Synthesis according to claim 1 2the method of nanometer bouquet, is characterized in that: the process of separate solid product is suction filtration, deionized water and absolute ethanol washing, drying, obtains product.
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CN107804873A (en) * 2017-11-20 2018-03-16 吉林大学 The method of the flower-shaped molybdenum disulfide electrode material of one step Hydrothermal Synthesiss and application
CN109174131A (en) * 2018-08-29 2019-01-11 厦门大学 The molybdenum disulfide nano floral material and its synthetic method of nickel cobalt modification and application
CN109261192A (en) * 2018-05-21 2019-01-25 淮阴师范学院 Attapulgite/g-C3N4/MoS2Heterojunction composite, preparation method and purposes
CN109465018A (en) * 2017-09-07 2019-03-15 中国科学院大连化学物理研究所 A kind of preparation method of nanoscale load type molybdenum sulfide catalyst
CN109569665A (en) * 2018-11-28 2019-04-05 东莞理工学院 A kind of preparation method and application of copper sulfide/vulcanization molybdenum composite material
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CN110776007A (en) * 2019-11-05 2020-02-11 北华航天工业学院 Preparation method of ping-pong chrysanthemum-shaped lithium vanadate material
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CN115974158A (en) * 2023-01-06 2023-04-18 四川轻化工大学 Hydrothermal method for synthesizing molybdenum disulfide by taking elemental sulfur as sulfur source

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CN107804873B (en) * 2017-11-20 2019-08-27 吉林大学 The method and application of the flower-shaped molybdenum disulfide electrode material of one step hydrothermal synthesis
CN107804873A (en) * 2017-11-20 2018-03-16 吉林大学 The method of the flower-shaped molybdenum disulfide electrode material of one step Hydrothermal Synthesiss and application
CN109261192B (en) * 2018-05-21 2020-07-17 淮阴师范学院 Attapulgite/g-C3N4/MoS2Heterojunction composite material, preparation method and application
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CN110339845A (en) * 2019-07-03 2019-10-18 西南大学 A kind of preparation method and liberation of hydrogen application of molybdenum disulfide flower-like nanometer ball
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CN110776007B (en) * 2019-11-05 2021-11-19 北华航天工业学院 Preparation method of ping-pong chrysanthemum-shaped lithium vanadate material
CN112551585A (en) * 2020-12-24 2021-03-26 齐鲁工业大学 Surfactant-induced MoS2Preparation method and application of nanoflower electrode material
CN114011438A (en) * 2021-11-29 2022-02-08 河南工程学院 High-exposure unsaturated sulfur atom MoS3Catalyst, preparation method and application
CN114011438B (en) * 2021-11-29 2023-09-01 河南工程学院 High-exposure unsaturated sulfur atom MoS 3 Catalyst, preparation method and application
CN114477103A (en) * 2022-01-20 2022-05-13 西安工业大学 MoS with high activity performance at room temperature2-xSexGrading gas-sensitive material and preparation method thereof
CN114477103B (en) * 2022-01-20 2023-10-24 西安工业大学 MoS with high activity at room temperature 2-x Se x Hierarchical gas-sensitive material and preparation method thereof
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