CN108751178A - A kind of carbonized graphite alkene and preparation method thereof - Google Patents
A kind of carbonized graphite alkene and preparation method thereof Download PDFInfo
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- CN108751178A CN108751178A CN201810747640.7A CN201810747640A CN108751178A CN 108751178 A CN108751178 A CN 108751178A CN 201810747640 A CN201810747640 A CN 201810747640A CN 108751178 A CN108751178 A CN 108751178A
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- graphite alkene
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/194—After-treatment
Abstract
The invention discloses a kind of carbonized graphite alkene and preparation method thereof, what the carbonized graphite alkene was made of the raw material of following weight parts:Glucose 30-40, ethyl cellulose 2-4, initiator 1-1.3, p-methyl benzenesulfonic acid 0.01-0.02, phosphorus trichloride 5-7, graphene oxide 160-200, sodium acrylate 60-70.Present invention introduces graphene oxides, intercalation modifying is carried out to graphene, carbon source is also introduced during intercalation, final high temperature is carbonized, stable dispersion of the carbon dust between graphene layer is realized, composite material of the invention has good mechanical stability, and functional higher, it is superior to be also used as materials, the comprehensive performances such as fire-retardant, absorption.
Description
Technical field
The invention belongs to field of graphene, and in particular to a kind of carbonized graphite alkene and preparation method thereof.
Background technology
Mesoporous material due to larger specific surface area, big hole hold and its manageable pore passage structure so that its
There is prodigious application in terms of ultracapacitor, but the electric conductivity of mesoporous material is poor, greatly limits their application;
Therefore, the purpose of the present invention is exactly between mesoporous material is introduced into graphene layer by way of intercalation, to
To stable graphene carbon powder composite material.
Invention content
In view of the defects and deficiencies of the prior art, the present invention intends to provide a kind of carbonized graphite alkene and its preparation sides
Method.
To achieve the above object, the present invention uses following technical scheme:
A kind of carbonized graphite alkene, it is made of the raw material of following weight parts:
Glucose 30-40, ethyl cellulose 2-4, initiator 1-1.3, p-methyl benzenesulfonic acid 0.01-0.02, phosphorus trichloride
5-7, graphene oxide 160-200, sodium acrylate 60-70.
The initiator is cumyl peroxide.
The preparation method of the carbonized graphite alkene, includes the following steps:
(1) initiator is taken, is added in the absolute ethyl alcohol of 20-30 times of its weight, stirs evenly, obtain initiator solution;
(2) glucose, ethyl cellulose, sodium acrylate mixing are taken, the deionized water of 10-15 times of mixture weight is added to
In, it stirs evenly, is sent in reaction kettle, be passed through nitrogen, it is 60-70 DEG C to adjust temperature of reaction kettle, insulated and stirred 4-5 hours,
Discharging cooling, obtains fibre-forming polymer solution;
(3) p-methyl benzenesulfonic acid, phosphorus trichloride mixing are taken, is added in the deionized water of 25-30 times of mixture weight, stirs
It mixes uniformly, is mixed with above-mentioned fibre-forming polymer solution, insulated and stirred 2-3 hours at 90-95 DEG C, graphene oxide, drop is added
Low temperature is 65-70 DEG C, 5-7 hours ultrasonic, filters, filter cake is washed, vacuum calcining:Vacuum degree is 8-10Pa, heating rate
For 70-90 DEG C/min, heat preservation roasting 10-12h after being warming up to 1050-1200 DEG C, natural cooling is to get the carbonized graphite alkene.
Advantages of the present invention:
The present invention is blended using glucose, ethyl cellulose as carbon source with sodium acrylate monomers, gathers under initiator effect
It closes, obtains fibre-forming polymer solution, later by the esterification of phosphorus trichloride and alcohol, obtain phosphate modified polyacrylic acid
Then sodium introduces graphene oxide, carry out intercalation modifying to graphene, carbon source, final high temperature carbon are also introduced during intercalation
Change, realize stable dispersion of the carbon dust between graphene layer, composite material of the invention has good mechanical stability, and work(
It is superior to be also used as materials, the comprehensive performances such as fire-retardant, absorption for energy property higher;The present invention composite material particularly suitable for
Ultracapacitor field, with larger specific surface area, big hole holds and its manageable pore passage structure, and conductive stability
Good, comprehensive performance is superior.
Specific implementation mode
Embodiment 1
A kind of carbonized graphite alkene, it is made of the raw material of following weight parts:
Glucose 40, ethyl cellulose 4, initiator 1.3, p-methyl benzenesulfonic acid 0.02, phosphorus trichloride 7, graphene oxide
200, sodium acrylate 70.
The initiator is cumyl peroxide.
The preparation method of the carbonized graphite alkene, includes the following steps:
(1) initiator is taken, is added in the absolute ethyl alcohol of 30 times of its weight, is stirred evenly, obtain initiator solution;
(2) glucose, ethyl cellulose, sodium acrylate mixing are taken, is added in the deionized water of 15 times of mixture weight,
It stirs evenly, is sent in reaction kettle, be passed through nitrogen, it is 70 DEG C to adjust temperature of reaction kettle, insulated and stirred 5 hours, discharging cooling,
Obtain fibre-forming polymer solution;
(3) p-methyl benzenesulfonic acid, phosphorus trichloride mixing are taken, is added in the deionized water of 30 times of mixture weight, stirs
Uniformly, it is mixed with above-mentioned fibre-forming polymer solution, insulated and stirred 3 hours at 95 DEG C, graphene oxide is added, reducing temperature is
70 DEG C, ultrasound 7 hours is filtered, filter cake is washed, vacuum calcining:Vacuum degree is 10Pa, and heating rate is 90 DEG C/min, heating
Heat preservation roasting 12h after to 1200 DEG C, natural cooling is to get the carbonized graphite alkene.
Embodiment 2
A kind of carbonized graphite alkene, it is made of the raw material of following weight parts:
Glucose 30-40, ethyl cellulose 2, initiator 1, p-methyl benzenesulfonic acid 0.01, phosphorus trichloride 5, graphene oxide
160, sodium acrylate 60.
The initiator is cumyl peroxide.
The preparation method of the carbonized graphite alkene, includes the following steps:
(1) initiator is taken, is added in the absolute ethyl alcohol of 20 times of its weight, is stirred evenly, obtain initiator solution;
(2) glucose, ethyl cellulose, sodium acrylate mixing are taken, is added in the deionized water of 10 times of mixture weight,
It stirs evenly, is sent in reaction kettle, be passed through nitrogen, it is 60 DEG C to adjust temperature of reaction kettle, insulated and stirred 4 hours, discharging cooling,
Obtain fibre-forming polymer solution;
(3) p-methyl benzenesulfonic acid, phosphorus trichloride mixing are taken, is added in the deionized water of 25 times of mixture weight, stirs
Uniformly, it is mixed with above-mentioned fibre-forming polymer solution, insulated and stirred 2 hours at 90 DEG C, graphene oxide is added, reducing temperature is
65 DEG C, ultrasound 5 hours is filtered, filter cake is washed, vacuum calcining:Vacuum degree is 8Pa, and heating rate is 70 DEG C/min, is warming up to
Heat preservation roasting 10h after 1050 DEG C, natural cooling is to get the carbonized graphite alkene.
Performance test:
Specific surface area:592-601m2/g;
Electrochemical property test:
In the koh electrolytic solution of 2mol/l, it is 298-314F/g that its specific volume is tested at 0.2A/g.
Claims (3)
1. a kind of carbonized graphite alkene, which is characterized in that it is made of the raw material of following weight parts:
Glucose 30-40, ethyl cellulose 2-4, initiator 1-1.3, p-methyl benzenesulfonic acid 0.01-0.02, phosphorus trichloride 5-7,
Graphene oxide 160-200, sodium acrylate 60-70.
2. a kind of carbonized graphite alkene according to claim 1, which is characterized in that the initiator is peroxidating diisopropyl
Benzene.
3. a kind of preparation method of carbonized graphite alkene as described in claim 1, which is characterized in that include the following steps:
(1) initiator is taken, is added in the absolute ethyl alcohol of 20-30 times of its weight, stirs evenly, obtain initiator solution;
(2) glucose, ethyl cellulose, sodium acrylate mixing are taken, is added in the deionized water of 10-15 times of mixture weight,
It stirs evenly, is sent in reaction kettle, be passed through nitrogen, it is 60-70 DEG C to adjust temperature of reaction kettle, insulated and stirred 4-5 hours, discharging
It is cooling, obtain fibre-forming polymer solution;
(3) p-methyl benzenesulfonic acid, phosphorus trichloride mixing are taken, is added in the deionized water of 25-30 times of mixture weight, stirring is equal
It is even, it is mixed with above-mentioned fibre-forming polymer solution, insulated and stirred 2-3 hours at 90-95 DEG C, graphene oxide is added, reduces temperature
Degree is 65-70 DEG C, 5-7 hours ultrasonic, filters, filter cake is washed, vacuum calcining:Vacuum degree is 8-10Pa, heating rate 70-
90 DEG C/min, heat preservation roasting 10-12h after being warming up to 1050-1200 DEG C, natural cooling is to get the carbonized graphite alkene.
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Cited By (1)
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CN110391419A (en) * | 2019-07-26 | 2019-10-29 | 广东工业大学 | A kind of porous carbon and its application in lithium-sulphur cell positive electrode |
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CN107359053A (en) * | 2017-06-21 | 2017-11-17 | 同济大学 | Graphene/carbon nano-cellulose complex carbon material and its preparation method and application |
CN107973283A (en) * | 2017-11-01 | 2018-05-01 | 华南理工大学 | A kind of elasticity carbon aerogels and its preparation method and application |
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WO2014168629A1 (en) * | 2013-04-12 | 2014-10-16 | General Electric Company | Membranes comprising graphene |
CN103950917A (en) * | 2014-05-07 | 2014-07-30 | 北京理工大学 | Method for preparing porous carbon material |
CN106467299A (en) * | 2016-06-27 | 2017-03-01 | 济南圣泉集团股份有限公司 | A kind of graphene-based multi-stage porous electric capacity charcoal and preparation method thereof and capacitor |
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