CN108054029A - A kind of preparation method of graphene melamine resin Hollow Sphere Composites - Google Patents
A kind of preparation method of graphene melamine resin Hollow Sphere Composites Download PDFInfo
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- CN108054029A CN108054029A CN201711389662.2A CN201711389662A CN108054029A CN 108054029 A CN108054029 A CN 108054029A CN 201711389662 A CN201711389662 A CN 201711389662A CN 108054029 A CN108054029 A CN 108054029A
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- Prior art keywords
- melamine resin
- graphite oxide
- graphene
- melamine
- hollow sphere
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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
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
-
- 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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- 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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- 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
- H01G11/32—Carbon-based
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
-
- 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
The invention discloses a kind of preparation methods of graphene/melamine resin Hollow Sphere Composites, it is related to Material Field, the present invention is using polyvinyl alcohol as dispersant, prepare monodispersed melamine resin medicine ball, with graphite oxide it is compound after, utilize high-temperature heat treatment method, graphene/melamine resin Hollow Sphere Composites have been synthesized for the first time, the charge and discharge under the current density of 1A/g, specific capacitance reach 625F/g, have many potential application prospects in electrode material for super capacitor field；Present invention process is simple, is suitble to scale industrial production.
Description
Technical field
The present invention relates to a kind of preparation methods of graphene melamine resin Hollow Sphere Composites, and it is compound to belong to special appearance
Technical field of material.
Background technology
Graphene is a kind of carbon material of sequential 2 D, it not only has larger specific surface area, but also its electric conductivity, electricity
Chemically, thermal stability, mechanicalness are excellent, therefore graphene is counted as a kind of electrode material of rationality.Due to graphene film
Between layer there is stronger π-π active forces, graphene sheet layer is made easily to reunite, so the graphene material actually prepared
Material, specific surface area are far below the theoretical value of single-layer graphene.
The number of plies and specific area size of grapheme material have the electro-chemical activity of material, the conductibility of electronics important
It influences.For graphene sheet layer is avoided to reunite, increase the specific surface area of grapheme material, forefathers are by graphene and other nano materials
It is compound.Really, there is relatively high specific capacitance as energy storage material these composite materials, but their production cost compared with
Height, cyclical stability, high rate performance are up for improving.Prepared by high-temperature heat treatment method have high specific capacitance graphene/melamine resin
Hollow ball hybrid supercapacitor material, has not yet to see report.
The content of the invention
To solve above-mentioned technical problem existing in the prior art, the present invention prepares graphene/close using high-temperature heat treatment method
Polyimide resin Hollow Sphere Composites provide a kind of side for the graphene-based hybrid supercapacitor material for preparing special appearance
Method.
To realize above-mentioned technical purpose, the technical solution adopted by the present invention is as follows：
A kind of preparation method of graphene melamine resin Hollow Sphere Composites, includes the following steps：
(1) formalin, melamine, hexa are added in reaction kettle to react under agitation,
The molar ratio of melamine and 37% formalin prepolymerization reaction, melamine and formaldehyde is 1:2-3, control ph 8-8.5,
85-105 DEG C of pre-polymerization temperature is controlled, the pre-polymerization time is 70-120min, and the quality of hexa is the 4- of melamine quality
12%；(2) add polyethylene glycol and carry out polycondensation reaction, control ph 5-6, the quality of polyethylene glycol is melamine quality
40-60%, wherein the molecular weight of polyethylene glycol be 800-1500；45-55 DEG C of condensation temperature is controlled, the polycondensation time is 80-
100min obtains melamine resin；
(3) graphite oxide is disperseed in deionized water, ultrasonic 1-6h, is made into the graphite oxide that concentration is 1mg/mL and disperses
Liquid；Melamine resin is added in deionized water, ultrasonic 0.5-3h, be made into the melamine resin dispersion liquid that concentration is 2.5mg/mL；
(4) under agitation, graphite oxide dispersion is mixed with melamine resin dispersion liquid, graphite oxide and melamine tree
The mass ratio of fat is 1:10-9:1,1-8h is continuously stirred, the two is made to be sufficiently mixed uniformly；Gained mixed solution is freezed
It is dry, obtain spongiform graphite oxide/melamine resin compound；
(5) under Ar gas shieldeds, with the heating rate of 0.5-5 DEG C/min, 400-900 DEG C is warming up to, carbonization time is
0.5-6h, rear cooled to room temperature obtain black graphene/melamine resin Hollow Sphere Composites.
It further limits, the graphite oxide dispersion ultrasonic time described in step (3) is 3h；The melamine resin point
Dispersion liquid ultrasonic time is 1.5h.
It further limits, the mass ratio of graphite oxide and melamine resin described in step (4) is 1:5；The oxygen
Graphite and melamine resin mixed liquor are stirred the time as 3h.
It further limits, the heating rate described in step (5) is 1 DEG C/min；The carburizing temperature is 600 DEG C；Institute
The carbonization time stated is 1h.
Advantageous effect：
(1) present invention prepares monodispersed melamine resin medicine ball, is answered with graphite oxide using polyvinyl alcohol as dispersant
After conjunction, using high-temperature heat treatment method, graphene/melamine resin Hollow Sphere Composites have been synthesized for the first time, it is close in the electric current of 1A/g
The lower charge and discharge of degree, specific capacitance reach 625F/g, have many potential application prospects in electrode material for super capacitor field；
(2) present invention process is simple, is suitble to scale industrial production.
Specific embodiment
In order to make those skilled in the art that the present invention may be better understood, with reference to embodiment to the technology of the present invention
Scheme further illustrates.
A kind of preparation method of graphene melamine resin Hollow Sphere Composites, includes the following steps：
(1) formalin, melamine, hexa are added in reaction kettle to react under agitation,
The molar ratio of melamine and 37% formalin prepolymerization reaction, melamine and formaldehyde is 1:2-3, control ph 8-8.5,
85-105 DEG C of pre-polymerization temperature is controlled, the pre-polymerization time is 70-120min, and the quality of hexa is the 4- of melamine quality
12%；
(2) add polyethylene glycol and carry out polycondensation reaction, control ph 5-6, the quality of polyethylene glycol is melamine matter
The molecular weight of the 40-60% of amount, wherein polyethylene glycol are 800-1500；45-55 DEG C of condensation temperature is controlled, the polycondensation time is 80-
100min obtains melamine resin；
(3) graphite oxide is disperseed in deionized water, ultrasonic 1-6h, is made into the graphite oxide that concentration is 1mg/mL and disperses
Liquid；Melamine resin is added in deionized water, ultrasonic 0.5-3h, be made into the melamine resin dispersion liquid that concentration is 2.5mg/mL；
(4) under agitation, graphite oxide dispersion is mixed with melamine resin dispersion liquid, graphite oxide and melamine tree
The mass ratio of fat is 1:10-9:1,1-8h is continuously stirred, the two is made to be sufficiently mixed uniformly；Gained mixed solution is freezed
It is dry, obtain spongiform graphite oxide/melamine resin compound；
(5) under Ar gas shieldeds, with the heating rate of 0.5-5 DEG C/min, 400-900 DEG C is warming up to, carbonization time is
0.5-6h, rear cooled to room temperature obtain black graphene/melamine resin Hollow Sphere Composites.
In preferred embodiment, the graphite oxide dispersion ultrasonic time described in step (3) is 3h；The melamine tree
Fat dispersion liquid ultrasonic time is 1.5h.
In preferred embodiment, the mass ratio of graphite oxide and melamine resin described in step (4) is 1:5；It is described
Graphite oxide and melamine resin mixed liquor, be stirred the time as 3h.
In preferred embodiment, the heating rate described in step (5) is 1 DEG C/min；The carburizing temperature is 600
℃；The carbonization time is 1h.
A kind of preparation method of graphene melamine resin Hollow Sphere Composites provided by the invention has been carried out in detail above
It is thin to introduce.The explanation of specific embodiment is only intended to help the method and its core concept for understanding the present invention.It should be pointed out that for
For those skilled in the art, without departing from the principle of the present invention, if can also be carried out to the present invention
Dry improvement and modification, these improvement and modification are also fallen into the protection domain of the claims in the present invention.
Claims (4)
1. the preparation method of a kind of graphene/melamine resin Hollow Sphere Composites, which is characterized in that include the following steps：
(1) formalin, melamine, hexa are added in reaction kettle to react under agitation, trimerization
The molar ratio of cyanamide and 37% formalin prepolymerization reaction, melamine and formaldehyde is 1:2-3, control ph 8-8.5, control
85-105 DEG C of pre-polymerization temperature, pre-polymerization time are 70-120min, and the quality of hexa is the 4- of melamine quality
12%；
(2) add polyethylene glycol and carry out polycondensation reaction, control ph 5-6, the quality of polyethylene glycol is melamine quality
The molecular weight of 40-60%, wherein polyethylene glycol are 800-1500；45-55 DEG C of condensation temperature is controlled, the polycondensation time is 80-
100min obtains melamine resin；
(3) graphite oxide is disperseed in deionized water, ultrasonic 1-6h, is made into the graphite oxide dispersion that concentration is 1mg/mL；
Melamine resin is added in deionized water, ultrasonic 0.5-3h, be made into the melamine resin dispersion liquid that concentration is 2.5mg/mL；
(4) under agitation, graphite oxide dispersion is mixed with melamine resin dispersion liquid, graphite oxide and melamine resin
Mass ratio is 1:10-9:1,1-8h is continuously stirred, the two is made to be sufficiently mixed uniformly；It is dry that gained mixed solution is subjected to freezing
It is dry, obtain spongiform graphite oxide/melamine resin compound；
(6) under Ar gas shieldeds, with the heating rate of 0.5-5 DEG C/min, 400-900 DEG C, carbonization time 0.5-6h is warming up to,
Cooled to room temperature afterwards obtains black graphene/melamine resin Hollow Sphere Composites.
2. a kind of preparation method of graphene/melamine resin Hollow Sphere Composites according to claim 1, feature exist
In the graphite oxide dispersion ultrasonic time described in step (3) is 3h；The melamine resin dispersion liquid ultrasonic time is
1.5h。
3. a kind of preparation method of graphene/melamine resin Hollow Sphere Composites according to claim 1, feature exist
In the mass ratio of graphite oxide and melamine resin described in step (4) is 1:5；The graphite oxide and melamine resin
Mixed liquor is stirred the time as 3h.
4. a kind of preparation method of graphene/melamine resin Hollow Sphere Composites according to claim 1, feature exist
In the heating rate described in step (5) is 1 DEG C/min；The carburizing temperature is 600 DEG C；The carbonization time is 1h.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711389662.2A CN108054029A (en) | 2017-12-21 | 2017-12-21 | A kind of preparation method of graphene melamine resin Hollow Sphere Composites |
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| CN201711389662.2A CN108054029A (en) | 2017-12-21 | 2017-12-21 | A kind of preparation method of graphene melamine resin Hollow Sphere Composites |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104167302A (en) * | 2014-08-26 | 2014-11-26 | 齐鲁工业大学 | Preparation method for grapheme/melamine resin hollow ball composite material |
| CN104804160A (en) * | 2015-05-04 | 2015-07-29 | 芜湖市宝艺游乐科技设备有限公司 | Environment-friendly oxidized graphene melamine resin and preparation method thereof |
| CN105218771A (en) * | 2015-10-29 | 2016-01-06 | 江苏润钰新材料科技有限公司 | A kind of preparation method of melmac |
-
2017
- 2017-12-21 CN CN201711389662.2A patent/CN108054029A/en not_active Withdrawn
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104167302A (en) * | 2014-08-26 | 2014-11-26 | 齐鲁工业大学 | Preparation method for grapheme/melamine resin hollow ball composite material |
| CN104804160A (en) * | 2015-05-04 | 2015-07-29 | 芜湖市宝艺游乐科技设备有限公司 | Environment-friendly oxidized graphene melamine resin and preparation method thereof |
| CN105218771A (en) * | 2015-10-29 | 2016-01-06 | 江苏润钰新材料科技有限公司 | A kind of preparation method of melmac |
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