CN108511206A - A kind of preparation method and application of melamine resin base carbon material electrode material for super capacitor - Google Patents
A kind of preparation method and application of melamine resin base carbon material electrode material for super capacitor Download PDFInfo
- Publication number
- CN108511206A CN108511206A CN201810262162.0A CN201810262162A CN108511206A CN 108511206 A CN108511206 A CN 108511206A CN 201810262162 A CN201810262162 A CN 201810262162A CN 108511206 A CN108511206 A CN 108511206A
- Authority
- CN
- China
- Prior art keywords
- melamine resin
- resin base
- base carbon
- carbon material
- super capacitor
- 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
Links
Classifications
-
- 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
- H01G11/44—Raw materials therefor, e.g. resins or coal
-
- 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 present invention relates to the preparation method and application that a kind of special appearance melamine resin base carbon material prepares electrode material for super capacitor.Its preparation process is as follows：A certain amount of melamine and formaldehyde are placed in three-necked flask first, stir 0.5h；Then 0.05 ~ 0.5g polyvinyl alcohol is dissolved in 90ml deionized waters, and glacial acetic acid is added；The product of above two step is mixed later, is reacted 5 ~ 10 minutes, obtained product is used into ethyl alcohol and deionized water alternating centrifugal, until after supernatant is neutral, is put into oven drying 8 hours；By obtained melamine resin under the protection of argon gas, 3 hours are carbonized at 600 ~ 800 DEG C to get a kind of special appearance melamine resin base carbon material.Preparation process of the present invention is simple, has controllability；The special appearance melamine resin base carbon material electrode material for super capacitor being prepared has many advantages, such as that stable structure, electrochemical performance, good cycle and specific capacitance are high, is highly suitable as electrode material and is applied to ultracapacitor field.
Description
Technical field
The invention belongs to new energy technical field of electronic materials, are related to a kind of melamine resin base carbon material super capacitor electrode
The preparation method and application of pole material.
Background technology
Melamine resin（MF）, chemical name melamine, English name melamine.It is that melamine reacts institute with formaldehyde
Obtained polymer has nitrogen content high, the advantages of can generating fake capacitance, increase specific capacitance and energy density.It can conduct
Presoma prepares nitrogenous active carbon material.
Song et al. activates the melamine resin after carbonization at 600 DEG C using KOH, then makes pyrroles after activation
Melamine resin surface aggregate has obtained the carbon material of the N doping of high power capacity holding.The material maintains after being recycled at 3000 times
94.3% high power capacity conservation rate.（Song L, Zou Y, Zhang H, et al. High Performance
Supercapacitor based on Polypyrrole /Melamine Formaldehyde Resin Derived
Carbon Material[J]. International Journal of Electrochemical Science, 2017,
12(2):1014-1024.）.Li et al. people has been pyrolyzed graphene（GN）The hollow melmac base carbon ball coated in sheet material
（HMCS）, the compound of 3D network structures has been obtained, a kind of electrode material for super capacitor that electrical property is relatively good has been obtained,
The specific capacitance of 0.2A/g is 720F/g（Li M, Zhang Y, Yang L, et al. Hollow melamine resin-
based carbon spheres/graphene composite with excellent performance for
supercapacitors[J]. Electrochimica Acta, 2015, 166:310-319.）.Bilal Khalid et al.
Pass through Na2CO3The colloidal sol of catalysis-gel polycondensation reaction is successfully prepared a kind of novel rich nitrogen porous graphene crosslinking melamine
Amine formaldehyde carbon gel has obtained the carbon jelly that nitrogen content is up to 14.29%（Khalid B, Meng Q, Li J, et al.
Nitrogen rich graphene-cross-linked melamine formaldehyde carbon cryogels for
supercapacitors[J]. Electrochimica Acta, 2014, 142:101-107.）.
Chinese patent literature CN105671692A discloses a kind of Nitrogen-rich porous carbon fiber electrode material that melamine resin is modified
The preparation method of material, includes the following steps：（1）It is 8.5 ~ 9.5 in the pH value of mixed system after melamine and formaldehyde are mixed
Under conditions of reacted, be added methanol after reaction, melamine resin be precipitated；（2）Polyacrylonitrile is dissolved in N, N- diformazans
Base formamide（DMF）In, melamine resin stirring and dissolving is added, spinning solution is made；（3）By spinning solution through high-voltage electrostatic spinning,
Obtain MF/PAN composite fibres；（4）By MF/PAN composite fibres through pre-oxidation treatment and carbonization treatment, it is fine that Nitrogen-rich porous carbon is made
Tie up electrode material.But this method obtained carbon material, when doing electrode material, specific capacitance is relatively low, when being electricity with the KOH of 6mol/L
Liquid is solved, constant-current discharge current density specific capacitance in 1A/g is only 125F/g.
Invention content
In view of the deficiencies of the prior art, the present invention provides a kind of specific capacitance height, the melamine resin base carbon of good cycle
The preparation method and application of material electrode material for super capacitor.
Technical scheme is as follows：
According to the present invention, a kind of preparation method of melamine resin base carbon material electrode material for super capacitor, including steps are as follows：
（1）1.8 ~ 3.8g melamines and 2 ~ 8ml formaldehyde are placed in three-necked flask, 0.5h is stirred；
（2）0.05 ~ 0.5g polyvinyl alcohol is dissolved in 90ml deionized waters；
（3）Step is added in the glacial acetic acid of 0.6 ~ 1.4ml（2）Obtained product；
（4）By step（3）Step is added in obtained product（1）In, it reacts 5 ~ 10 minutes, obtained product using ethyl alcohol and is gone
Ionized water alternating centrifugal is put into oven drying 8 hours until after supernatant is neutral；
（5）By step（4）Obtained melamine resin is carbonized 3 hours to get one kind under the protection of argon gas at 600 ~ 800 DEG C
Special appearance melamine resin base carbon material.
, according to the invention it is preferred to, step（1）Described in the dosage of melamine be 2.8g, the dosage of formaldehyde is
4.5ml。
, according to the invention it is preferred to, step（2）In polyvinyl alcohol dosage be 0.1g.
, according to the invention it is preferred to, step（3）In glacial acetic acid dosage be 1.2ml.
, according to the invention it is preferred to, step（4）Described in reaction time be 8min.
, according to the invention it is preferred to, step（5）Described in carburizing temperature be 750oC。
A kind of special appearance melamine resin base carbon material prepares electrode material for super capacitor, is used for ultracapacitor.
The technical advantage of the present invention is as follows：
(1) preparation process of the present invention is simple, has controllability, can control carbon material by controlling the dosage of polyvinyl alcohol
Specific surface area and shape characteristic；
(2) the melamine resin base carbon material electrode material for super capacitor that the present invention is prepared has stable structure, electrochemistry
It has excellent performance, the advantages that good cycle and specific capacitance are high, is highly suitable as electrode material and is applied to ultracapacitor
Field.
Description of the drawings
Fig. 1 is the scanning electron microscope of melamine resin base carbon material electrode material for super capacitor made from the embodiment of the present invention 1
Figure.
Fig. 2 is that the constant current of melamine resin base carbon material electrode material for super capacitor made from the embodiment of the present invention 1 fills
Electric discharge figure.
Specific implementation mode
With reference to specific embodiments and the drawings, the present invention is described further, but not limited to this.
Experimental method described in following embodiments is unless otherwise specified conventional method simultaneously；The reagent and material
Material, unless otherwise specified, commercially obtains.
Embodiment 1：
（1）2.8g melamines and 4.5ml formaldehyde are placed in three-necked flask, 0.5h is stirred；Then 0.1g polyvinyl alcohol is molten
1.2ml glacial acetic acid is added in 90ml deionized waters in solution；The product of above two step is mixed later, is reacted 8 minutes, will
The product arrived uses ethyl alcohol and deionized water alternating centrifugal, until after supernatant is neutral, is put into oven drying 8 hours；
（2）By obtained melamine resin under the protection of argon gas, 3 hours are carbonized at 750 DEG C to get a kind of special appearance melamine
Resin base carbon material.
The scanning electron microscope (SEM) photograph of melamine resin base carbon material electrode material for super capacitor made from this example as shown in Figure 1,
The lamellar structure that polymer is made of many fragments as shown in Figure 1.
Constant current charge-discharge such as Fig. 2 institutes of melamine resin base carbon material electrode material for super capacitor made from this example
Show, as shown in Figure 2, it is 253F/g that 1A/g, which measures specific capacitance, and it is 177F/g that 10A/g, which measures specific capacitance, and cyclical stability is excellent.
Embodiment 2：
（1）3.8g melamines and 5.5ml formaldehyde are placed in three-necked flask, 0.5h is stirred；Then 0.1g polyvinyl alcohol is molten
1.2ml glacial acetic acid is added in 90ml deionized waters in solution；The product of above two step is mixed later, is reacted 10 minutes, will
The product arrived uses ethyl alcohol and deionized water alternating centrifugal, until after supernatant is neutral, is put into oven drying 8 hours；
（2）By obtained melamine resin under the protection of argon gas, 3 hours are carbonized at 600 DEG C to get a kind of special appearance melamine
Resin base carbon material.
Using three-electrode system, using 2mol/L sulfuric acid solutions as electrolyte, it is 192F/g, 10A/g that 1A/g, which measures specific capacitance,
It is 30F/g to measure specific capacitance, and stability is poor.
Embodiment 3：
（1）2.8g melamines and 6.5ml formaldehyde are placed in three-necked flask, 0.5h is stirred；Then 0.2g polyvinyl alcohol is molten
0.6ml glacial acetic acid is added in 90ml deionized waters in solution；The product of above two step is mixed later, is reacted 5 minutes, will
The product arrived uses ethyl alcohol and deionized water alternating centrifugal, until after supernatant is neutral, is put into oven drying 8 hours；
（2）By obtained melamine resin under the protection of argon gas, 3 hours are carbonized at 750 DEG C to get a kind of special appearance melamine
Resin base carbon material.
Using three-electrode system, using 2mol/L sulfuric acid solutions as electrolyte, it is 202F/g, 10A/g that 1A/g, which measures specific capacitance,
It is 122F/g to measure specific capacitance, and stability is preferable.
Embodiment 4：
（1）1.8g melamines and 8ml formaldehyde are placed in three-necked flask, 0.5h is stirred；Then 0.5g polyvinyl alcohol is dissolved
In 90ml deionized waters, and 1.4ml glacial acetic acid is added；The product of above two step is mixed later, reacts 6 minutes, will obtain
Product use ethyl alcohol and deionized water alternating centrifugal, until after supernatant is neutral, be put into oven drying 8 hours；
（2）By obtained melamine resin under the protection of argon gas, 3 hours are carbonized at 800 DEG C to get a kind of special appearance melamine
Resin base carbon material.
Using three-electrode system, using 2mol/L sulfuric acid solutions as electrolyte, it is 182F/g, 10A/g that 1A/g, which measures specific capacitance,
It is 98F/g to measure specific capacitance, and stability is preferable.
Claims (6)
1. a kind of preparation method of melamine resin base carbon material electrode material for super capacitor, including steps are as follows：
（1）1.8 ~ 3.8g melamines and 2 ~ 8ml formaldehyde are placed in three-necked flask, 0.5h is stirred；
（2）0.05 ~ 0.5g polyvinyl alcohol is dissolved in 90ml deionized waters；
（3）Step is added in the glacial acetic acid of 0.6 ~ 1.4ml（2）Obtained product；
（4）By step（3）Step is added in obtained product（1）In, it reacts 5 ~ 10 minutes, obtained product using ethyl alcohol and is gone
Ionized water alternating centrifugal is put into oven drying 8 hours until after supernatant is neutral；
（5）By step（4）Obtained melamine resin is carbonized 3 hours to get one kind under the protection of argon gas at 600 ~ 800 DEG C
Special appearance melamine resin base carbon material.
2. the preparation method of melamine resin base carbon material electrode material for super capacitor according to claim 1, feature
It is, step（1）In the dosage of melamine be 2.8g, the dosage of formaldehyde is 4.5ml.
3. the preparation method of melamine resin base carbon material electrode material for super capacitor according to claim 1, feature
It is, step（2）In polyvinyl alcohol dosage be 0.1g.
4. the preparation method of melamine resin base carbon material electrode material for super capacitor according to claim 1, feature
It is, step（3）In glacial acetic acid dosage be 1.2ml.
5. the preparation method of melamine resin base carbon material electrode material for super capacitor according to claim 1, feature
It is, step（4）Described in reaction time be 8min.
6. the preparation method of melamine resin base carbon material electrode material for super capacitor according to claim 1, feature
It is, step（5）Described in carburizing temperature be 750oC。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810262162.0A CN108511206A (en) | 2018-03-28 | 2018-03-28 | A kind of preparation method and application of melamine resin base carbon material electrode material for super capacitor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810262162.0A CN108511206A (en) | 2018-03-28 | 2018-03-28 | A kind of preparation method and application of melamine resin base carbon material electrode material for super capacitor |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108511206A true CN108511206A (en) | 2018-09-07 |
Family
ID=63378883
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810262162.0A Pending CN108511206A (en) | 2018-03-28 | 2018-03-28 | A kind of preparation method and application of melamine resin base carbon material electrode material for super capacitor |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108511206A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109704305A (en) * | 2019-01-22 | 2019-05-03 | 齐鲁工业大学 | It is a kind of using ZIF-67 as the preparation method and application of templated synthesis melamine resin base Carbon Materials |
| CN109824920A (en) * | 2019-01-22 | 2019-05-31 | 齐鲁工业大学 | One-step method prepares polyvinyl alcohol copolymer melamine resin nanosphere |
| CN110828196A (en) * | 2019-10-24 | 2020-02-21 | 暨南大学 | Shape-controllable carbonized melamine resin supercapacitor electrode material and preparation method and application thereof |
Citations (2)
| 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 |
| 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 |
-
2018
- 2018-03-28 CN CN201810262162.0A patent/CN108511206A/en active Pending
Patent Citations (2)
| 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 |
| 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 |
Non-Patent Citations (1)
| Title |
|---|
| MEI LI ET AL: "Hollow melamine resin-based carbon spheres/graphene composite with excellent performance for supercapacitors", 《ELECTROCHIMICA ACTA》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109704305A (en) * | 2019-01-22 | 2019-05-03 | 齐鲁工业大学 | It is a kind of using ZIF-67 as the preparation method and application of templated synthesis melamine resin base Carbon Materials |
| CN109824920A (en) * | 2019-01-22 | 2019-05-31 | 齐鲁工业大学 | One-step method prepares polyvinyl alcohol copolymer melamine resin nanosphere |
| CN109704305B (en) * | 2019-01-22 | 2022-03-18 | 齐鲁工业大学 | Preparation method and application of melamine resin-based carbon material synthesized by taking ZIF-67 as template |
| CN110828196A (en) * | 2019-10-24 | 2020-02-21 | 暨南大学 | Shape-controllable carbonized melamine resin supercapacitor electrode material and preparation method and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105761950B (en) | A kind of preparation method of porous rich nitrogen carbon fiber electrode | |
| CN104332640B (en) | Thermal reduction graphene oxide/carbon nano-fiber method for preparing composite electrode used for all-vanadium redox flow battery | |
| CN105839228B (en) | A kind of preparation method of polyacrylonitrile-radical conductive fiber material | |
| CN104466134B (en) | The preparation method of self-supporting graphene/carbon nano-tube hybrid foam support amino anthraquinones base polymer | |
| CN107256956A (en) | A kind of nitrogen-doped carbon cladding vanadium nitride electrode material and preparation method and application | |
| CN101985358A (en) | Method for quickly preparing carbon-silicon dioxide composite aerogel | |
| CN108511206A (en) | A kind of preparation method and application of melamine resin base carbon material electrode material for super capacitor | |
| CN108054020B (en) | Preparation method and application of nitrogen-doped carbon particle/graphitized carbon-nitrogen composite material | |
| CN106340401A (en) | Preparing method of composite electrode material and application thereof | |
| CN104392847A (en) | Preparation method of morphology controllable metal oxide/active carbon fiber combination electrode material | |
| CN105789575A (en) | Silicon dioxide carbon composite negative electrode material, modified silicon dioxide carbon composite negative electrode material and preparation methods and application of silicon dioxide carbon composite negative electrode material and modified silicon dioxide carbon composite negative electrode material | |
| CN104167303A (en) | Mesopore vanadium oxide/carbon composite nano material and preparation method thereof | |
| CN108922790A (en) | A kind of manganese dioxide/N doping porous carbon composite preparation method and application of sodium ion insertion | |
| CN112695413B (en) | MXene/porous carbon nanofiber composite material and preparation method and application thereof | |
| CN111883366A (en) | Polypyrrole nanosphere @ titanium carbide composite material and preparation method and application thereof | |
| CN108711518A (en) | Porous carbon nanobelts of nitrogen oxygen codope and its preparation method and application | |
| CN110407194A (en) | The hollow Nano carbon balls of three-dimensional porous N doping and its controllable method for preparing and application | |
| CN105504277A (en) | Highly-ordered porous graphene/polyaniline composite material and preparation method thereof | |
| CN110911175B (en) | Carbonized eggshell membrane, MXene and polypyrrole composite gel and preparation method and application thereof | |
| CN104743543B (en) | A kind of preparation method of polyaniline/phenolic aldehyde base material with carbon element | |
| CN105261485B (en) | A kind of preparation method of capacitor electrode material | |
| CN109326453B (en) | Polypyrrole supercapacitor composite electrode material and preparation method thereof | |
| CN110112014A (en) | A kind of carbon fabric-polypyrrole combination electrode material and its preparation method and application | |
| CN111430153B (en) | Carbon nano aerogel material for all-solid-state supercapacitor and preparation method and application thereof | |
| CN107217482B (en) | A kind of polyaniline hybridized electrode material of nitrogen-phosphor codoping porous carbon membrane@and preparation method thereof with interface covalent linkage |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180907 |
|
| RJ01 | Rejection of invention patent application after publication |