CN106423218A - Synthesis method of molybdenum disulfide/carbon nano composite material - Google Patents

Synthesis method of molybdenum disulfide/carbon nano composite material Download PDF

Info

Publication number
CN106423218A
CN106423218A CN201610849294.4A CN201610849294A CN106423218A CN 106423218 A CN106423218 A CN 106423218A CN 201610849294 A CN201610849294 A CN 201610849294A CN 106423218 A CN106423218 A CN 106423218A
Authority
CN
China
Prior art keywords
composite material
carbon nano
solution
molybdenum bisuphide
carbon
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201610849294.4A
Other languages
Chinese (zh)
Inventor
耿芹
杨超
宿新泰
梁小玉
闫宝林
陈航
赵云龙
张敏
王吉德
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Xinjiang University
Original Assignee
Xinjiang University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Xinjiang University filed Critical Xinjiang University
Priority to CN201610849294.4A priority Critical patent/CN106423218A/en
Publication of CN106423218A publication Critical patent/CN106423218A/en
Pending legal-status Critical Current

Links

Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J27/00Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/02Sulfur, selenium or tellurium; Compounds thereof
    • B01J27/04Sulfides
    • B01J27/047Sulfides with chromium, molybdenum, tungsten or polonium
    • B01J27/051Molybdenum
    • B01J35/40
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures

Abstract

The invention discloses a synthesis method of a molybdenum disulfide/carbon composite material for preparing potassium humate, belonging to the field of inorganic non-metal materials. The method comprises the following steps: dissolving a soluble molybdenum salt ammonium molybdate tetrahydrate in water, adding potassium humate into the solution, reversely dropping the mixed solution into nitric acid, and regulating the pH value to 1-3 to prepare a precipitate; and roasting in argon or any other inert atmosphere by a fused salt roasting process to generate carbon thermal reaction, thereby obtaining the composite structure on which nanorods with the length of 100nm or so are carried on the carbon film. The method has the advantages of simple technique and low cost. The biomass material potassium humate is used as the carbon source to directly synthesize the loaded nano composite structure.

Description

A kind of synthetic method of molybdenum bisuphide/carbon nano-composite material
Technical field
The invention belongs to new inorganic non-metallic materials research and development technology field, specifically disclose one kind and be related to molybdenum bisuphide/carbon and receive The co-precipitation of nano composite material and the synthetic method of fuse salt roasting.
Background technology
Molybdenum bisuphide has the layer structure of similar graphite and stable physicochemical properties, is widely used in solid lubrication Agent, hydrogen storage material, battery electrode material, catalysis material etc..Nanometer class molybdenum disulfide material, because its high adsorption capacity, catalysis are anti- The feature such as active height should be used as coal liquefaction, coal pyrolysis, hydrodesulfurization, the catalyst of sulphur removal denitrification in oil.But by Little in nanoparticle size, surface energy is high, is susceptible to reunite between particle, nano material dispersion in media as well and steady Determine to become one of subject matter limiting it in commercial Application.In order to improve the reunion of nano molybdenum disulfide particle, in recent years, stone Black alkene or graphene oxide become the focus that people study.At present, method predominantly organic tool stripping method, the reduction of Graphene are prepared The synthetic methods such as graphite oxide method, epitaxial growth method and metal catalysed processes.However, graphenic surface assumes stable inertia, indissoluble Solution is in solvent it more difficult to equably be combined with other organic or inorganic materials.Therefore, prepare graphene composite material, be mostly First graphene oxide is combined with nano material, then will compound after material reduction obtain graphene composite material.This preparation Complex steps, product property is often difficult to meet application demand, therefore, it is necessary to exploitation one kind directly obtains graphene-supported list The preparation method of dispersing nanoparticles.
Prepare at present nano particle/graphite alkene main method have chemical reduction method, electrochemical deposition method, thermal evaporation, Hydro-thermal method, sol-gel process etc..Some researchs show, select suitable carbon source and synthesis condition can directly obtain the stone of load Black alkene.Humic acidss are a kind of natural macromolecular organic compound, are mainly adopted the side of " alkali extraction and acid precipitation " by weathered coal or brown coal Method obtains.Humic acidss have uncertain molecular weight, contain multiple work such as carboxyl, hydroxyl, phenolic hydroxyl group, quinonyl, methoxyl group thereon Property functional group.It has the functions such as good absorption, complexation, exchange.
Content of the invention
The purpose of the present invention is:In order to prove to select suitable carbon source, molybdenum bisuphide/carbon can be directly obtained nano combined Material.Propose using humic acidss essence potassium complexing metal molybdenum ion, further by roasting after itself and sodium sulfate mixed grinding, preparation The method of molybdenum bisuphide/carbon nano-composite material.
The technical scheme is that:A kind of synthetic method of molybdenum bisuphide/carbon nano-composite material, this synthetic method bag Include following steps:(1)The four hydration Ammoniun Heptamolybdate Solution 40ml of configuration 0.25M, then it is added thereto to 2g humic acidss essence potassium, by two Person is mixed and stirred for into mixed solution, standby;(2)The salpeter solution 100ml of configuration 0.5M, by step(1)Middle stirring obtains Mixed solution is dropwise added drop-wise in the salpeter solution of 0.5M, and the pH adjusting solution is between 1-3, and standing was sunk after a period of time Starch, standby;(3)By step(2)In the precipitate lyophilizing for preparing, press 1 with anhydrous sodium sulfate:10 mass ratio mixing is ground Mill, under Ar gas atmosphere, under the conditions of 600 DEG C or 700 DEG C or 800 DEG C, with the heating gradient roasting 3h of 10 DEG C/min, naturally cold But arrive room temperature, obtain the presoma of molybdenum bisuphide/carbon nano-composite material, standby;(4)By step(3)In the presoma that obtains With water and each centrifuge washing of dehydrated alcohol five times, it is finally stored in dehydrated alcohol;Product is dried to obtain at 50 DEG C two sulfur Change the powder body of molybdenum/carbon nano-composite material.Using the feature of humic acidss essence potassium " alkali extraction and acid precipitation ", adopt in fuse salt roasting system With humic acidss essence this biological material of potassium as carbon source synthesis of carbon/molybdenum disulfide/carbon nano-composite material, described potassium humate purchase Buy from Xinjiang Shuan Long humic acidss company.
Beneficial effect:The invention provides a kind of method directly obtaining molybdenum bisuphide/carbon nano-composite material, using from The humic acidss essence this not only cheap but also efficient biological material of potassium extracting in weathered coal, as carbon source, is realized at utmost The utilization of resources, be finally reached environmental conservation, the purpose of resource higher value application.
Brief description
Fig. 1:The X-ray of molybdenum bisuphide/carbon nano-composite material when T=600 DEG C of preparation method of the present invention(XRD) collection of illustrative plates;
Fig. 2:The transmission electron microscope figure spectrum of molybdenum bisuphide/carbon nano-composite material when T=600 DEG C of preparation method of the present invention (TEM);
From the X-ray collection of illustrative plates of Fig. 1 it is recognised that the material obtaining when T=600 DEG C is molybdenum bisuphide/carbon nano-composite material.From Molybdenum bisuphide/carbon nano-composite material obtained by the image of the transmission electron microscope of Fig. 2 can be seen that is 100nm Nanometer rods be uniformly supported on the pattern on carbon film surface.It is therefore seen that, select suitable carbon source-humic acidss essence potassium, permissible Directly obtain molybdenum bisuphide/carbon nano-composite material.
Specific embodiment
The embodiment 1, (NH of configuration 0.25M4)6Mo7O24·4H2O solution 40ml, then it is added thereto to 2g humic acidss essence potassium, It is reconfigured at the HNO of 0.5M3Solution 100ml.Under conditions of magnetic agitation, by (NH4)6Mo7O24·4H2O is mixed with humic acidss essence potassium Close solution and be slowly reversely added drop-wise to HNO3In solution.After above turbid solution is stood, suction out the water on upper strata, then precipitate is entered Row lyophilizing, takes the humic acidss after 1g lyophilizing essence potassium-molybdic acid presoma and 10g anhydrous sodium sulfate with 1:10 mass ratio is mixed Grind, then under Ar gas atmosphere, under the conditions of 600 DEG C, with 10 DEG C/min heating gradient roasting 3h, naturally cool to room temperature, then Respectively sample is carried out with water and ethanol with each five times of centrifuge washing, in ethanol by sample preservation, 50 DEG C of drying obtain sulfur finally Change molybdenum/carbon nano-composite material
The embodiment 2, (NH of configuration 0.25M4)6Mo7O24·4H2O solution 40ml, then it is added thereto to 2g humic acidss essence potassium, then join Set to 0 the HNO of .5M3Solution 100ml.Under conditions of magnetic agitation, by (NH4)6Mo7O24·4H2O mixes molten with humic acidss essence potassium Liquid is slowly reversely added drop-wise to HNO3In solution.After above turbid solution is stood, suction out the water on upper strata, then precipitate is frozen Dry, take the essence potassium-molybdic acid presoma of the humic acidss after 1g lyophilizing and 10g anhydrous sodium sulfate with 1:10 mass ratio carries out mixing and grinds Mill, then under Ar gas atmosphere, under the conditions of 700 DEG C, with 10 DEG C/min heating gradient roasting 3h, naturally cools to room temperature, uses water With ethanol, respectively sample is carried out with each five times of centrifuge washing, finally in ethanol by sample preservation, 50 DEG C of drying obtain molybdenum sulfide/ Carbon nano-composite material.
The embodiment 3, (NH of configuration 0.25M4)6Mo7O24·4H2O solution 40ml, then it is added thereto to 2g humic acidss essence potassium, It is reconfigured at the HNO of 0.5M3Solution 100ml.Under conditions of magnetic agitation, by (NH4)6Mo7O24·4H2O is mixed with humic acidss essence potassium Close solution and be slowly reversely added drop-wise to HNO3In solution.After above turbid solution is stood, suction out the water on upper strata, then precipitate is entered Row lyophilizing, takes the humic acidss after 1g lyophilizing essence potassium-molybdic acid presoma and 10g anhydrous sodium sulfate with 1:10 mass ratio is mixed Grind, then under Ar gas atmosphere, under the conditions of 800 DEG C, with 10 DEG C/min heating gradient roasting 3h, naturally cool to room temperature, then Respectively sample is carried out with water and ethanol with each five times of centrifuge washing, in ethanol by sample preservation, 50 DEG C of drying obtain sulfur finally Change molybdenum/carbon nano-composite material.
Potassium humate used by above-mentioned experiment is bought from Xinjiang Shuan Long humic acidss company.
Conclusion:By selecting suitable carbon source-humic acidss essence potassium, directly obtain molybdenum bisuphide/carbon nano-composite material, Its pattern be 100 nm about nanometer rods be uniformly supported on carbon film surface.
The main technical content of the present invention is with Ammonium Molybdate Tetrahydrate and cheap humic acidss essence potassium mixed solution as raw material, Back titration, in nitric acid, is obtained precipitation.Again with anhydrous sodium sulfate mixed grinding, using fuse salt roasting method, anti-through carbon heat Should, using anhydrous sodium sulfate both as template agent, and as sulphur source, obtain 100nm about nanometer rods be uniformly supported on carbon Molybdenum bisuphide/carbon nano-composite material on film surface.

Claims (2)

1. a kind of synthetic method of molybdenum bisuphide/carbon nano-composite material, this synthetic method comprises the following steps:
(1)Configuration 0.25M tetra- hydration ammonium heptamolybdate 40ml, then it is added thereto to 2g humic acidss essence potassium, both are mixed and stirred for Become mixed solution, standby;
(2)Configure the salpeter solution 100ml of 0.5 M, by step(1)The mixed solution that middle stirring obtains dropwise is added drop-wise to 0.5M's In salpeter solution, the pH adjusting solution is between 1-3, and standing is precipitated thing after a period of time, standby;
(3)By step(2)In the precipitate lyophilizing for preparing, press 1 with anhydrous sodium sulfate:10 quality than mixed grinding, in Ar Under gas atmosphere, under the conditions of 600 DEG C or 700 DEG C or 800 DEG C, with the heating gradient roasting 3h of 10 DEG C/min, naturally cool to room Temperature, obtains the presoma of molybdenum bisuphide/carbon nano-composite material, standby;
(4)By step(3)In the presoma water that obtains and each centrifuge washing of dehydrated alcohol five times, be finally stored in dehydrated alcohol In;Product is dried to obtain at 50 DEG C the powder body of molybdenum bisuphide/carbon nano-composite material.
2. the method that coprecipitation according to claim 1 prepares molybdenum bisuphide/carbon nano-composite material, its feature exists In:Described potassium humate is bought from Xinjiang Shuan Long humic acidss company.
CN201610849294.4A 2016-09-26 2016-09-26 Synthesis method of molybdenum disulfide/carbon nano composite material Pending CN106423218A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610849294.4A CN106423218A (en) 2016-09-26 2016-09-26 Synthesis method of molybdenum disulfide/carbon nano composite material

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610849294.4A CN106423218A (en) 2016-09-26 2016-09-26 Synthesis method of molybdenum disulfide/carbon nano composite material

Publications (1)

Publication Number Publication Date
CN106423218A true CN106423218A (en) 2017-02-22

Family

ID=58169410

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201610849294.4A Pending CN106423218A (en) 2016-09-26 2016-09-26 Synthesis method of molybdenum disulfide/carbon nano composite material

Country Status (1)

Country Link
CN (1) CN106423218A (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111014249A (en) * 2019-12-24 2020-04-17 青岛大学 Preparation method of two-dimensional transition metal chalcogenide-carbon composite material
CN111370675A (en) * 2020-03-24 2020-07-03 合肥工业大学 Carbon nanosheet sodium-ion battery cathode material inlaid with metal phosphide and preparation method thereof
CN113981489A (en) * 2021-10-28 2022-01-28 济南大学 Molybdenum carbide/carbon composite material, preparation method based on molten salt method and application

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103641117A (en) * 2013-12-17 2014-03-19 中国科学院新疆理化技术研究所 Method for preparing activated carbon material with humic acid as raw material and application of activated carbon material
US9314777B2 (en) * 2012-07-27 2016-04-19 Lawrence Livermore National Security, Llc High surface area graphene-supported metal chalcogenide assembly
CN105858713A (en) * 2016-04-01 2016-08-17 新疆大学 Molten salt roasting method for synthesis of supported nanocomposite

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9314777B2 (en) * 2012-07-27 2016-04-19 Lawrence Livermore National Security, Llc High surface area graphene-supported metal chalcogenide assembly
CN103641117A (en) * 2013-12-17 2014-03-19 中国科学院新疆理化技术研究所 Method for preparing activated carbon material with humic acid as raw material and application of activated carbon material
CN105858713A (en) * 2016-04-01 2016-08-17 新疆大学 Molten salt roasting method for synthesis of supported nanocomposite

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
WEI FU 等: "In situ catalytic growth of large-area multilayered graphene/MoS2 heterostructures", 《SCIENTIFIC REPORTS》 *
耿芹 等: "二硫化钼/碳复合材料的制备及其电化学性能研究", 《中国化学会第30届学术年会-第三十分会:化学电源》 *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111014249A (en) * 2019-12-24 2020-04-17 青岛大学 Preparation method of two-dimensional transition metal chalcogenide-carbon composite material
CN111014249B (en) * 2019-12-24 2021-09-21 青岛大学 Preparation method of two-dimensional transition metal chalcogenide-carbon composite material
CN111370675A (en) * 2020-03-24 2020-07-03 合肥工业大学 Carbon nanosheet sodium-ion battery cathode material inlaid with metal phosphide and preparation method thereof
CN111370675B (en) * 2020-03-24 2022-09-13 合肥工业大学 Carbon nanosheet sodium ion battery cathode material inlaid with metal phosphide and preparation method thereof
CN113981489A (en) * 2021-10-28 2022-01-28 济南大学 Molybdenum carbide/carbon composite material, preparation method based on molten salt method and application

Similar Documents

Publication Publication Date Title
CN105845910B (en) Flower-shaped MoS2@graphene nanocomposite material and preparation method thereof
Li et al. Advanced MoS2 and graphene heterostructures as high-performance anode for sodium-ion batteries
CN105417581A (en) Method for complexing hydrothermal synthesis of uniform flower-like MoS2 nanospheres
Zhong et al. Controllable synthesis of hierarchical MoS2 nanotubes with ultra-uniform and superior storage potassium properties
Zeng et al. Enhancement of electrochemical performance by the oxygen vacancies in hematite as anode material for lithium-ion batteries
Huang et al. Defective ZnCo2O4 with Zn vacancies: synthesis, property and electrochemical application
CN101186290A (en) Anode material vanadium lithium phosphate and preparation method thereof
CN104821238A (en) Method for preparing electrode material molybdate for super capacitor and application thereof
CN106423218A (en) Synthesis method of molybdenum disulfide/carbon nano composite material
CN105329946A (en) Molybdenum disulfide nanosheet with rich active sites as well as preparation method and application of molybdenum disulfide nanosheet
CN106145190A (en) The preparation method of a kind of molybdenum disulfide nano tube and the application in lithium ion battery thereof
Su et al. MnO QD/graphene dot fabrics: a versatile nanohybrid material
Yi et al. Hollow mesoporous MnO/MnS/SiC/S-CN composites prepared from soda pulping black liquor for lithium-ion batteries
Liu et al. Spraying Coagulation‐Assisted Hydrothermal Synthesis of MoS2/Carbon/Graphene Composite Microspheres for Lithium‐Ion Battery Applications
Xin et al. Coupling Mo2C@ C core-shell nanocrystals on 3D graphene hybrid aerogel for high-performance lithium ion battery
CN105712404A (en) Preparation method of MoS2 quantum dots
McNulty et al. The effect of particle size, morphology and C-rates on 3D structured Co3O4 inverse opal conversion mode anode materials
CN105609769A (en) Preparation method for multi-level structured molybdenum disulfide microsphere negative electrode material of lithium battery
Bindumadhavan et al. Ultrafine CoO embedded reduced graphene oxide nanocomposites: a high rate anode for Li–ion battery
CN103682340A (en) Iron-based fluoride nano material with hierarchical structure, preparation method and application thereof
CN107428535B (en) Lithium manganese phosphate nanoparticles, method for producing same, carbon-coated lithium manganese phosphate nanoparticles, carbon-coated lithium manganese phosphate nanoparticle granules, and lithium ion battery
CN105161678B (en) A kind of MULTILAYER COMPOSITE titania nanotube material for electrode of lithium cell
Rajasekhara Reddy et al. Construction of an Ultra‐High‐Energy Density Hybrid Supercapacitor with Self‐Assembled 3D Hydrangea Flower‐like Mo‐rich CoMoO4 Microstructures
CN113097468B (en) C/CoSe 2 Preparation method and application of @ NC composite material
Yu et al. Zinc–cobalt bimetallic sulfide anchored on the surface of reduced graphene oxide used as anode for lithium ion battery

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication

Application publication date: 20170222

RJ01 Rejection of invention patent application after publication