CN108305789A - A kind of preparation method of polyacrylonitrile/molybdenum disulfide composite material for ultracapacitor - Google Patents
A kind of preparation method of polyacrylonitrile/molybdenum disulfide composite material for ultracapacitor Download PDFInfo
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- CN108305789A CN108305789A CN201711481492.0A CN201711481492A CN108305789A CN 108305789 A CN108305789 A CN 108305789A CN 201711481492 A CN201711481492 A CN 201711481492A CN 108305789 A CN108305789 A CN 108305789A
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- pan
- pmma
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- deionized water
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/48—Conductive polymers
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
A kind of disclosure of the invention preparation method of polyacrylonitrile/molybdenum disulfide composite material for ultracapacitor.By Sodium Molybdate Dihydrate (Na2MoO4·2H2O), thiocarbamide (CH4N2S it) is uniformly mixed with polymethyl methacrylate/polyacrylonitrile (PMMA/PAN) nucleocapsid, the high temperature cabonization after hydro-thermal reaction obtains MoS2/ PAN composite materials.Preparation method disclosed by the invention forms the PAN hollow spheres structures with uniform macropore using PMMA as template, and grows MoS on the surfaces PAN2Nano flower had not only facilitated transporting for electrolyte ion, but also had higher specific surface area, advantageously formed electric double layer.And entirely preparation process is simple, and it is environmentally protective.
Description
Technical field
The present invention relates to electrochemical technology fields, and in particular to ultracapacitor field, more particularly to it is a kind of for super
The preparation method of the polyacrylonitrile of capacitor/molybdenum disulfide composite material.
Background technology
The chemical property of electrode material for super capacitor is usually restricted by Multiple factors, such as specific surface area, aperture
Distribution, electric conductivity etc..First, specific surface area is bigger, and the electrolyte ion of absorption is more, can store more energy.Its
Secondary, pore size and structure can also influence the formation of electric double layer.Only sizeable aperture allows electrolyte ion to enter,
Electrode material surface could be infiltrated and form electric double layer.And complicated pore passage structure can also influence electrolyte ion in duct
Patency.The present invention mainly improves super capacitor from two above angle in conjunction with the characteristic of polyacrylonitrile and molybdenum disulfide
The chemical property of device electrode material.
Molybdenum disulfide (MoS2) it is used as a kind of transient metal sulfide, there is the layer structure of similar graphite, and physics
Chemical property is stablized.By long-term scientific research, the different nanoscale MoS of pattern is successfully prepared by a variety of methods2
Particle.
Invention content
The present invention is to improve the chemical property of electrode material for super capacitor, is provided a kind of for ultracapacitor
The preparation method of polyacrylonitrile/molybdenum disulfide electrode composite material.
One aspect of the present invention provides a kind of preparation side of polyacrylonitrile/molybdenum disulfide composite material for ultracapacitor
Method includes the following steps:
A. the nucleocapsid of polymetylmethacrylate/polyacrylonitrile (PAN) is prepared comprising following steps：
A-1. methyl methacrylate MMA and potassium peroxydisulfate KPS are add to deionized water, are stirred under nitrogen atmosphere
For a period of time；
A-2. the solution, acrylonitrile AN and potassium peroxydisulfate KPS of step A-1 is taken to be add to deionized water, in nitrogen atmosphere
Lower stirring a period of time；
A-3. the PMMA/PAN solution of step A-2 is centrifuged, is cleaned for several times and dried with deionized water, obtains PMMA/PAN
Nucleocapsid；
B. by PMMA/PAN nucleocapsids above-mentioned and Sodium Molybdate Dihydrate (Na2MoO4·2H2O), thiocarbamide (CH4N2S it) mixes,
It carries out hydro-thermal reaction and obtains MoS2/PMMA/PAN；
C. the MoS that high temperature cabonization step B is obtained2/ PMMA/PAN removes PMMA, obtains MoS2/ PAN composite materials.
In technical scheme of the present invention, step A-1, and A-2. is stirred 2-4 hours under 60-80 DEG C of nitrogen atmosphere.
In technical scheme of the present invention, the specific method is as follows by step B：
B-1. Sodium Molybdate Dihydrate and thiocarbamide (mass ratio 1 are weighed:2) powder is added in deionized water and stirs evenly；
B-2. it weighs the PMMA/PAN powder in step A-3 and deionized water, ultrasonic agitation is added；And PMMA/PAN powder and
The mass ratio of Sodium Molybdate Dihydrate is 1:10-1:50.
B-3. by step B-1 and step B-2 solution mix ultrasonic mixing it is uniform after, hydro-thermal is anti-at 120-200 DEG C
It answers；
B-4. it is filtered by vacuum, is cleaned for several times and dried with deionized water, obtain MoS2/PMMA/PAN。
In technical scheme of the present invention, the specific method is as follows by step C：By MoS2/ PMMA/PAN powder is mixed in hydrogen argon
It under atmosphere after 600-800 DEG C of heating a period of time, is cleaned with ethyl alcohol and deionized water, vacuum filtration obtains MoS2/PAN。
In technical scheme of the present invention, the specific method is as follows by step A：
A-1. 5-10ml methyl methacrylate MMA and 5-10mg potassium peroxydisulfates KPS is added to 100-300ml deionizations
In water, stirred 3-5 hours under 60-80 DEG C of nitrogen atmosphere with magnetic stirrer；
A-2. the solution of 100-200ml steps A-1,4-15ml acrylonitrile AN and 1-10mg potassium peroxydisulfates KPS is taken to be added to
In 50-200ml deionized waters, stirred 2-4 hours under 60-80 DEG C of nitrogen atmosphere with magnetic stirrer；
A-3. the PMMA/PAN solution of step A-2 is centrifuged, is cleaned with deionized water for several times and dry.
In technical scheme of the present invention, the specific method is as follows by step B：
B-1. Sodium Molybdate Dihydrate and thiocarbamide (mass ratio 1 are weighed:2) powder be added in deionized water stir it is 30 minutes -1 small
When；
B-2. it weighs the PMMA/PAN powder in step A-3 and deionized water is added, it is 1-2 hours ultrasonic；And PMMA/PAN powder
The mass ratio of end and Sodium Molybdate Dihydrate is 1:10-1:50.
B-3. it is poured into reaction kettle after the solution in step B-1 and step B-2 being mixed ultrasound 1-2 hours, in 120-200
Hydro-thermal reaction 8-24 hours at DEG C；
B-4. the mixed solution in vacuum filtration step B-3 is cleaned for several times and is dried with deionized water, obtains MoS2/
PMMA/PAN。
In technical scheme of the present invention, the specific method is as follows by step C：
C-1. by MoS2The 600-800 DEG C of heating 30 under hydrogen (5%) argon (95%) mixed gas atmosphere of/PMMA/PAN powder
- 2 hours minutes；
C-2. it is filtered by vacuum with the powder obtained in ethyl alcohol and deionized water cleaning step C-1 respectively and is obtained MoS2/PAN。
The second aspect of the present invention provide a kind of polyacrylonitrile for ultracapacitor being prepared such as the above method/
Molybdenum disulfide composite material.
The third aspect of the present invention provides a kind of ultracapacitor, and structure includes：The positive and negative pole housing of capacitor, diaphragm,
Electrolyte, shrapnel, steel disc, positive and negative anodes current collector, positive and negative pole material, the positive and negative pole material are porous electrode material above-mentioned
Material.
Polyacrylonitrile prepared by the present invention/molybdenum disulfide composite material, being formed as template using PMMA is had uniformly greatly
The PAN hollow spheres structures in hole, and grow MoS on the surfaces PAN2Nano flower had not only facilitated transporting for electrolyte ion, but also had higher
Specific surface area, advantageously form electric double layer.And entirely preparation process is simple, and it is environmentally protective.
Wherein, using the globe daisy shape MoS of Hydrothermal Growth2Because having higher specific surface area to can be applied to ultracapacitor
Electrode material, and preparation process have be easy to control, product grain uniformly, advantages of environment protection.With polymethyl
Sour methyl esters PMMA is the hollow beads of PAN of template construct, and structure-controllable, uniform pore diameter transports convenient for electrolyte ion.With MoS2
In conjunction with helping to improve the transfer efficiency of ion, increase effective ratio area, and then improve the electrochemistry of electric double layer capacitance entirety
Performance
Description of the drawings
Attached drawing is to be used to provide further understanding of the present invention, and become part of specification, with the present invention's
Embodiment explains the present invention jointly, does not limit the invention.In the accompanying drawings,
Fig. 1 is one of polyacrylonitrile of the present invention/molybdenum disulfide composite material preparation flow figure.In figure, 1 it is PAN, 2 is
PMMA, 3 are MoS2。
Specific implementation mode
The specific embodiment of the invention is described below in conjunction with attached drawing.
Embodiment 1
(1) 5ml methyl methacrylate MMA and 5mg potassium peroxydisulfates KPS is added in 150ml deionized waters, uses magnetic force
Blender stirs 4 hours under 75 DEG C of nitrogen atmospheres；
(2) solution of 50ml steps (1), 4ml acrylonitrile AN and 4mg potassium peroxydisulfates KPS is taken to be added to 100ml deionized waters
In, it is stirred 2 hours under 70 DEG C of nitrogen atmospheres with magnetic stirrer；
(3) the PMMA/PAN solution of step (2) is centrifuged, is cleaned with deionized water for several times and dry.
(4) 0.3g Sodium Molybdate Dihydrates are weighed and 0.6g thiocarbamide powder is added in 40ml deionized waters and stirs 30 minutes；
(5) it weighs the PMMA/PAN powder in 30mg steps (3) and 20ml deionized waters, ultrasound 1 hour is added；
(6) it is poured into reaction kettle after the solution in step (4) and step (5) being mixed ultrasound 1 hour, the water at 180 DEG C
Thermal response 12 hours；
(7) mixed solution in vacuum filtration step (6) is cleaned for several times and dry with deionized water；
(8) by the powder in step (7) under hydrogen (5%) argon (95%) mixed gas atmosphere 700 DEG C heat 30 minutes；
(9) powder obtained respectively with ethyl alcohol and deionized water cleaning step (8), vacuum filtration obtain MoS2/ PAN is compound
Material；
(10) substance obtained in step (9) is mixed to be dissolved in N-Methyl pyrrolidone with Kynoar, carbon black and is made
At slurry, the mass ratio of active material, bonding agent and conductive agent is 8:1:1.
(11) slurry made from step (10) is coated in nickel foam, and is dried in vacuo 24 hours under 80 DEG C of environment.
(12) nickel foam in step (11) is washed into pole piece with the punching pin of a diameter of 13um.
(13) it is assembled into button ultracapacitor according to the sequence of anode cover, pole piece, diaphragm, pole piece, shrapnel and negative electrode casing,
In an assembling process, few drops of electrolyte are added.
The basic principles, main features and advantages of the present invention have been shown and described above.The technology of the industry
For personnel it should be appreciated that the present invention is not limited by examples detailed above, described in examples detailed above and specification is to illustrate the present invention
Principle, various changes and improvements may be made to the invention without departing from the spirit and scope of the present invention, these variation and
Improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention is by appended claims and its is equal
Object defines.
Claims (6)
1. a kind of preparation method of polyacrylonitrile/molybdenum disulfide composite material for ultracapacitor, includes the following steps:
A. the nucleocapsid of PMMA/PAN is prepared comprising following steps：
A-1. PMMA and KPS are add to deionized water, under nitrogen atmosphere stirring a period of time；
A-2. the solution, AN and KPS of step A-1 is taken to be add to deionized water, under nitrogen atmosphere stirring a period of time；
A-3. the PMMA/PAN solution of step A-2 is centrifuged, is cleaned for several times and dried with deionized water, obtains PMMA/PAN nucleocapsids
Structure；
B. by PMMA/PAN nucleocapsids above-mentioned and Na2MoO4·2H2O、CH4N2S is mixed, and is carried out hydro-thermal reaction and is obtained MoS2/
PMMA/PAN；
C. the MoS that high temperature cabonization step B is obtained2/ PMMA/PAN removes PMMA, obtains MoS2/ PAN composite materials.
2. preparation method according to claim 1, which is characterized in that step A-1, and A-2. is in 60-80 DEG C of nitrogen
It is stirred 2-4 hours under atmosphere.
3. preparation method according to claim 1, which is characterized in that the specific method is as follows by step B：
B-1. Na is weighed2MoO4·2H2O and CH4N2S powder, mass ratio 1:2, it is added in deionized water and stirs evenly；
B-2. it weighs the PMMA/PAN powder in step A-3 and deionized water, ultrasonic agitation is added；And PMMA/PAN powder and
Na2MoO4·2H2The mass ratio of O is 1:10-1:50.
B-3. by step B-1 and step B-2 solution mix ultrasonic mixing it is uniform after, the hydro-thermal reaction at 120-200 DEG C；
B-4. it is filtered by vacuum, is cleaned for several times and dried with deionized water, obtain MoS2/PMMA/PAN。
4. preparation method according to claim 1, which is characterized in that the specific method is as follows by step C：By MoS2/PMMA/
PAN powder after 600-800 DEG C of heating a period of time, is cleaned, vacuum under hydrogen-argon-mixed body atmosphere with ethyl alcohol and deionized water
Suction filtration obtains MoS2/PAN。
5. a kind of polypropylene for ultracapacitor being prepared such as the claims 1-4 any one of them methods
Nitrile/molybdenum disulfide composite material.
6. a kind of ultracapacitor, structure include：The positive and negative pole housing of capacitor, diaphragm, electrolyte, shrapnel, steel disc, positive and negative anodes
Current collector, positive and negative pole material, the positive and negative pole material are the polypropylene that claim 1-4 any one of them methods are prepared
Nitrile/molybdenum disulfide composite material.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109731549A (en) * | 2019-02-26 | 2019-05-10 | 东北电力大学 | Adsorbed film is blended in MoS2-PAN |
| CN113314351A (en) * | 2021-05-14 | 2021-08-27 | 上海工程技术大学 | Polyacrylonitrile-based boron carbon nitrogen nanofiber electrode material and preparation method and application thereof |
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