CN108133833A - A kind of preparation process of graphene melamine resin composite material - Google Patents
A kind of preparation process of graphene melamine resin composite material Download PDFInfo
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- CN108133833A CN108133833A CN201711389827.6A CN201711389827A CN108133833A CN 108133833 A CN108133833 A CN 108133833A CN 201711389827 A CN201711389827 A CN 201711389827A CN 108133833 A CN108133833 A CN 108133833A
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- melamine resin
- graphite oxide
- graphene
- composite material
- preparation process
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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
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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
- H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
-
- 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
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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 processes of graphene melamine resin composite material, 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 processes of graphene melamine resin composite material, belong to special appearance composite material system
Standby technical field.
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.
Invention content
To solve above-mentioned technical problem of the existing technology, 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 the above-mentioned technical purpose, the technical solution adopted by the present invention is as follows：
A kind of preparation process of graphene melamine resin composite material, includes the following steps：
(1) it is melamine to be calculated according to molar ratio：Formaldehyde：Distilled water is 1：2.0-2.7：The ratio of 4-5, by melamine
Control speed of agitator is 500r/ after amine, formaldehyde and distilled water are added in container and are heated to 75-80 DEG C after being uniformly mixed
Min is stirred reaction 0.3-0.4h, obtains reaction solution；
(2) pH for the reaction solution for adjusting above-mentioned gained with triethanolamine solution is 8-9, is continued controlled at 75-80
DEG C, rotating speed 500r/min, until transparent obtaining melamine resin solution；
(3) by graphite oxide dispersion in deionized water, ultrasonic 1-6h is made into the graphite oxide dispersion of a concentration of 1mg/mL
Liquid；Melamine resin is added in deionized water, ultrasonic 0.5-3h, be made into the melamine resin dispersion liquid of a concentration of 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；
(6) 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.
(1) it is melamine to be calculated according to molar ratio：Formaldehyde：Distilled water is 1：2.0-2.7：The ratio of 4-5, by melamine
Control speed of agitator is 500r/ after amine, formaldehyde and distilled water are added in container and are heated to 75-80 DEG C after being uniformly mixed
Min is stirred reaction 0.3-0.4h, obtains reaction solution；
(2) pH for the reaction solution for adjusting above-mentioned gained with triethanolamine solution is 8-9, is continued controlled at 75-80
DEG C, rotating speed 500r/min, until transparent obtaining melamine resin solution；
(3) by graphite oxide dispersion in deionized water, ultrasonic 1-6h is made into the graphite oxide dispersion of a concentration of 1mg/mL
Liquid；Melamine resin is added in deionized water, ultrasonic 0.5-3h, be made into the melamine resin dispersion liquid of a concentration of 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；
(6) 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 process of graphene melamine resin composite material provided by the invention is described in detail above.
The explanation of specific embodiment is merely used to help understand the method and its core concept of the present invention.It should be pointed out that for this technology
For the those of ordinary skill in field, without departing from the principle of the present invention, several improvement can also be carried out to the present invention
And modification, these improvement and modification are also fallen within the protection scope of the claims of the present invention.
Claims (4)
1. a kind of preparation process of graphene melamine resin composite material, which is characterized in that include the following steps：
(1) it is melamine to be calculated according to molar ratio：Formaldehyde：Distilled water is 1：2.0-2.7：The ratio of 4-5, by melamine,
Control speed of agitator is 500r/min after formaldehyde and distilled water are added in container and are heated to 75-80 DEG C after being uniformly mixed
Reaction 0.3-0.4h is stirred, obtains reaction solution；
(2) pH for the reaction solution for adjusting above-mentioned gained with triethanolamine solution is 8-9, continue controlled at 75-80 DEG C, turn
Fast 500r/min obtains melamine resin solution until transparent；
(3) by graphite oxide dispersion in deionized water, ultrasonic 1-6h is made into the graphite oxide dispersion of a concentration of 1mg/mL；
Melamine resin is added in deionized water, ultrasonic 0.5-3h, be made into the melamine resin dispersion liquid of a concentration of 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.
A kind of 2. preparation process of graphene melamine resin composite material according to claim 1, which is characterized in that step
(3) the graphite oxide dispersion ultrasonic time described in is 3h；The melamine resin dispersion liquid ultrasonic time is 1.5h.
A kind of 3. preparation process of graphene melamine resin composite material according to claim 1, which is characterized in that step
(4) mass ratio of graphite oxide and melamine resin described in is 1:5；The graphite oxide and melamine resin mixed liquor,
The time is stirred as 3h.
A kind of 4. preparation process of graphene melamine resin composite material according to claim 1, which is characterized in that step
(5) heating rate described in 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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| CN201711389827.6A CN108133833A (en) | 2017-12-21 | 2017-12-21 | A kind of preparation process of graphene melamine resin composite material |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711389827.6A CN108133833A (en) | 2017-12-21 | 2017-12-21 | A kind of preparation process of graphene melamine resin composite material |
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| CN201711389827.6A Withdrawn CN108133833A (en) | 2017-12-21 | 2017-12-21 | A kind of preparation process of graphene melamine resin composite material |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5317689A (en) * | 1976-07-31 | 1978-02-17 | Matsushita Electric Works Ltd | Preparation of urea-melamine resins |
| CN103464068A (en) * | 2013-09-06 | 2013-12-25 | 上海应用技术学院 | Pressure-sensitive melamine resin essence microcapsule and preparation method thereof |
| CN104167302A (en) * | 2014-08-26 | 2014-11-26 | 齐鲁工业大学 | Preparation method for grapheme/melamine resin hollow ball composite material |
| CN105671692A (en) * | 2016-02-05 | 2016-06-15 | 扬州大学 | Preparation method of melamine resin modified nitrogen-rich porous carbon fiber electrode material |
-
2017
- 2017-12-21 CN CN201711389827.6A patent/CN108133833A/en not_active Withdrawn
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5317689A (en) * | 1976-07-31 | 1978-02-17 | Matsushita Electric Works Ltd | Preparation of urea-melamine resins |
| CN103464068A (en) * | 2013-09-06 | 2013-12-25 | 上海应用技术学院 | Pressure-sensitive melamine resin essence microcapsule and preparation method thereof |
| CN104167302A (en) * | 2014-08-26 | 2014-11-26 | 齐鲁工业大学 | Preparation method for grapheme/melamine resin hollow ball composite material |
| CN105671692A (en) * | 2016-02-05 | 2016-06-15 | 扬州大学 | Preparation method of melamine resin modified nitrogen-rich porous carbon fiber electrode material |
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