CN108773842A - A kind of preparation method and graphene of graphene - Google Patents
A kind of preparation method and graphene of graphene Download PDFInfo
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- CN108773842A CN108773842A CN201811041931.0A CN201811041931A CN108773842A CN 108773842 A CN108773842 A CN 108773842A CN 201811041931 A CN201811041931 A CN 201811041931A CN 108773842 A CN108773842 A CN 108773842A
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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
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G81/00—Macromolecular compounds obtained by interreacting polymers in the absence of monomers, e.g. block polymers
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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
- C01B2204/00—Structure or properties of graphene
- C01B2204/04—Specific amount of layers or specific thickness
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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
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/22—Electronic properties
Abstract
The present invention provides a kind of preparation method of graphene and graphenes, graphite powder is uniformly mixed by the preparation method with intercalator first, using mechanical lapping mode, obtain mixing presoma, mixing presoma obtained is mixed with organic solvent then, the poly-dopamine modified through sulfhydrylation hydroxyethyl starch, dispersant are sequentially added, after stirring evenly, it is ultrasonically treated, obtains graphite ene product.The preparation method of graphene of the present invention is avoided using solution in the prior art expansion stripping, and use the relatively mild poly-dopamine modified through sulfhydrylation hydroxyethyl starch and dispersant is removed, wherein, the poly-dopamine of sulfhydrylation hydroxyethyl starch modification, with special surface-active, the strong adsorption capacity shown, π-pi-electron cloud that can be between the benzene ring structure of graphite generates absorption, to which the outermost graphene of natural graphite is fallen to from graphite substrate in solvent, graphene product is obtained.
Description
Technical field
The invention belongs to grapheme material preparing technical fields, and in particular to a kind of preparation method and graphite of graphene
Alkene.
Background technology
Graphene is by sp2The monoatomic layer two-dimensional material that hydbridized carbon atoms are arranged to make up.Monoatomic layer two-dimensional material stone
Black alkene not only has the characteristics that transparent, light and flexible, is most thin, the most hard nano material being currently known, and has
There are many other excellent properties, for example the thermal coefficient of graphene is about 5300W/mK, higher than natural graphite, carbon nanotube and
The materials such as diamond；Electron mobility under graphene room temperature is more than 15000cm2/ Vs is higher than carbon nanotubes and silicon crystal；
The conductivity of graphene is up to 10-6S/m, it is lower than copper or silver, it is the highest material of current conductivity.These characteristics of graphene
So that it is in lithium ion battery, ultracapacitor, solar cell, sea water desalination, light emitting diode, sensor, hydrogen storage, catalysis
The fields such as agent carrier, composite material, coating, biologic bracket material, drug controlled release have wide practical use.
Currently, the preparation method of graphene mainly have mechanical stripping method, chemical vapour deposition technique, epitaxial crystal growth method and
Oxidation-reduction method etc..Wherein, mechanical stripping method is to obtain pure graphene sheet body using mechanical stripping graphite, but because yield is too low
And it can not be mass produced；Chemical vapour deposition technique or epitaxial crystal flop-in method are to utilize hydrocarbonization for being passed through thermal cracking
It closes object air source and is deposited on nickel sheet or copper sheet to prepare graphene, characteristic is that can prepare large area single-layer or multi-layer graphite
Alkene, but its disadvantage is that uniformity is difficult to control with thickness；In addition, in growing graphene on insulator base material, such as in silicon carbide
Surface can grow very thin graphene, and it is expensive and is difficult to prepare large area；Oxidation-reduction method, then be using graphite powder or
Graphite fibre generates functionalized graphite's oxide with the strong oxidizers such as sulfuric acid and nitric acid or the chemical stripping of other oxidation processes, then
Using high temperature furnace with 1100 DEG C to 1250 DEG C of high temperature, graphite oxide composite is made to expand stripping rapidly, although graphite oxide
Can be stripped to form graphene oxide, but the physics and electronic structure due to graphene are adversely affected, stone
The electric conductivity of black oxide is more much lower than graphene, and the processing procedure time is long, and the graphene after reduction is easily deformed and sticks up
It is bent so that graphene quality is very different.
For this purpose, Chinese patent literature CN107973293A provides a kind of preparation method and graphene of graphene, system
Preparation Method is that graphene is prepared by way of three rank strippings, and the three ranks stripping is followed successively by single order graphite mechanical stripping and inserts
Layer, second order solution expansion stripping and the stripping of three rank ultrasounds, wherein single order graphite mechanical stripping and intercalation are that graphite and intercalation are situated between
Matter mixes, and mechanically, graphite is carried out a degree of stripping and intercalation, obtains graphene presoma；Second order solution
Plavini stripping detaches graphene, and will be with defective graphene to be added graphene presoma into strong acid solution
Interlayer is further opened, and Activated Graphite alkene dispersion liquid is obtained；The stripping of three rank ultrasounds is further to surpass Activated Graphite alkene dispersion liquid
Sound is removed, and the graphene dispersing solution that lamellar spacing is small, the number of plies is few is obtained.But used second order solution is swollen in above-mentioned preparation method
There is the defect for the chemical bonding structure for destroying graphene obtained in swollen stripping so that the electronic conductivity of obtained graphene compared with
It is low, influence further applying for graphene.Therefore, how the preparation method of existing graphene is improved to subtract as far as possible
The destruction of the chemical bonding structure of few graphene improves the electron conduction of graphene obtained, this carrys out those skilled in the art
Say it is technical barrier urgently to be resolved hurrily.
Invention content
The present invention provides a kind of preparation method of graphene, and the graphene which is prepared has preferable electricity
Sub- performance, electronic conductivity is higher, and further provides the graphene being prepared by the preparation method.
The present invention solve the technical solution that uses of above-mentioned technical problem for:
The first aspect of the present invention provides a kind of preparation method of graphene, includes the following steps:
(1) graphite powder is uniformly mixed with intercalator, using mechanical lapping mode, obtains mixing presoma；
(2) step (1) mixing presoma obtained is mixed with organic solvent, is sequentially added through sulfhydrylation ethoxy
The poly-dopamine of starch modification, dispersant after stirring evenly, carry out ultrasound, obtain graphite ene product.
In the preparation method of above-mentioned graphene, the preparation method of the poly-dopamine through the modification of sulfhydrylation hydroxyethyl starch
It is as follows:
(1) it by hydroxyethyl starch carboxylated under alkaline condition, is then reacted with 2- (two sulphur of pyridine)-ethylamine hydrochloride
To hydroxyethyl starch -2- (two sulphur of pyridine)；
(2) hydroxyethyl starch -2- made from the step (1) (two sulphur of pyridine) sulfhydrylation sulfhydrylation ethoxy is obtained to form sediment
Powder；
(3) sulfhydrylation hydroxyethyl starch made from the step (2) mixed with poly-dopamine and anti-under alkaline condition
It should obtain the poly-dopamine modified by sulfhydrylation hydroxyethyl starch.
In the preparation method of above-mentioned graphene, it is preferable that in the step (3), the sulfhydrylation hydroxyethyl starch and institute
The mass ratio for stating poly-dopamine is 5:1；The pH of the alkaline condition is 10, and the reaction time is 30h.
In the preparation method of above-mentioned graphene, in the step (1), by hydroxyethyl starch carboxylated under alkaline condition
The specific steps are：Hydroxyethyl starch is dissolved in deionized water, sodium hydroxide and monoxone are sequentially added and is carried out at 100 DEG C
Reaction.
In the preparation method of above-mentioned graphene, in the step (1), it is preferable that the graphite powder is crystalline flake graphite, expansion
Graphite or amorphous graphite；The intercalator is sodium carbonate, sodium bicarbonate or sodium sulfite.
Preferably, the mass ratio of the graphite powder and the intercalator is 1:(3~10), preferably 1：(5~8).
In the preparation method of above-mentioned graphene, in the step (1),
The mechanical lapping mode is horizontal grinding, planetary grinding or high-energy ball milling, the mechanical lapping mode when
Between be 50~150h.
Preferably, the graphite powder and the poly-dopamine through the modification of sulfhydrylation hydroxyethyl starch, the dispersant
Mass ratio is 1:(10~50):(30~80), preferably 1:30:50.
Preferably, the dispersant is neopelex or polyvinylpyrrolidone；The organic solvent is first
Alcohol, ethyl alcohol or isopropanol.
Second aspect of the present invention provides a kind of graphene that above-mentioned preparation method is prepared.
The above-mentioned technical proposal of the present invention has the following advantages that:
(1) graphite powder is uniformly mixed, using machinery by the preparation method of graphene of the present invention with intercalator first
Lapping mode obtains mixing presoma, then mixes mixing presoma obtained with organic solvent, sequentially add through sulfhydrylation
The poly-dopamine of hydroxyethyl starch modification, dispersant, after stirring evenly, are ultrasonically treated, obtain graphite ene product.The present invention
The preparation method of the graphene is avoided using solution in the prior art expansion stripping, and is used relatively mild through mercapto
The poly-dopamine and dispersant of base hydroxyethyl starch modification are removed, wherein sulfhydrylation hydroxyethyl starch is modified poly- more
Bar amine, has a special surface-active, the strong adsorption capacity shown, π-that can be between the benzene ring structure of graphite
Pi-electron cloud generates absorption, to which the outermost graphene of natural graphite is fallen to from graphite substrate in solvent, by constantly heavy
This multiple process, hardly destroys the chemical bonding structure of graphene, obtains graphene product.
Specific implementation mode
Technical scheme of the present invention will be clearly and completely described below, it is clear that described embodiment is this hair
Bright a part of the embodiment, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not having
There is the every other embodiment obtained under the premise of making creative work, shall fall within the protection scope of the present invention.In addition, below
Involved technical characteristic as long as they do not conflict with each other can be mutual in described different embodiments of the present invention
In conjunction with.
In the present invention, raw materials used is commercially available product.
Embodiment 1
The preparation method for the poly-dopamine modified through sulfhydrylation hydroxyethyl starch is present embodiments provided, including is walked as follows
Suddenly：
(1) the hydroxyethyl starch 1g that molecular weight is 25000Da, ethoxy degree of substitution is 0.5 is taken to be dissolved in 10mL deionized waters
In, then stirring sequentially adds 1.2g sodium hydroxides and 1.5g monoxones and forms reaction system to dissolving, and by the reaction system
Reaction 5h is carried out at 100 DEG C, stops reaction, and cold room temperature processed pours into reaction system in 20mL methanol, stirs, and centrifugation obtains
White precipitate, the as hydroxyethyl starch of carboxylated；
It takes the hydroxyethyl starch of 0.8g carboxylated obtained above to be dissolved in 10mL deionized waters, 250mg1- (3- bis- is added
Methylaminopropyl) -3- ethyl-carbodiimide hydrochlorides, 75mgN- HOSu NHSs and 150mg 2- (two sulphur of pyridine)-second
Amine hydrochlorate forms reaction system, this reaction system is stirred to react 30h in 30 DEG C, centrifuges, and supernatant is taken to use molecular cut off
For the bag filter deionized water dialysis 3 days of 3500Da, freeze-drying obtains hydroxyethyl starch -2- (two sulphur of pyridine)；
(2) it takes hydroxyethyl starch -2- made from 0.5g above-mentioned steps (two sulphur of pyridine) to be dissolved in 10mL dimethyl sulfoxides, is added
420mg dithiothreitol (DTT)s are stirred at room temperature reaction for 24 hours, then use molecular cut off for the dialysis of 3500Da under nitrogen protection
Bag deionized water dialysis 3 days, freeze-drying obtain sulfhydrylation hydroxyethyl starch；
(3) it takes 40mg poly-dopamines to be dispersed in 10mL deionized waters, stirs ultrasound 30min, sodium hydroxide is added and adjusts
PH is 10, is then slowly added to sulfhydrylation hydroxyethyl starch side made from 200mg above-mentioned steps and stirs, after addition, in room
30h is stirred to react under temperature, to remove unreacted sulfhydrylation hydroxyethyl starch, the molecular cut off of above-mentioned super filter tube is for ultrafiltration
100kDa, ultrafiltration rotating speed are 4000 revs/min, obtain the poly-dopamine modified by sulfhydrylation hydroxyethyl starch.
Embodiment 2
The preparation method of graphene provided in this embodiment includes the following steps:
(1) 1g crystalline graphite powders are uniformly mixed with 10g sodium bicarbonates and carry out horizontal grinding 50h, grinding is finished, mixed
Close presoma；
(2) step (1) mixing presoma obtained is mixed with 250mL methanol, then sequentially adds 10g through sulfydryl
Poly-dopamine, the 80g neopelexes for changing hydroxyethyl starch modification, after stirring evenly, are surpassed with ultrasonic generator
Sonication, ultrasonic time 1h, ultrasonic power 300W obtain graphite ene product then through washing, centrifugation, 50 DEG C of dryings；
The poly-dopamine modified through sulfhydrylation hydroxyethyl starch used in the present embodiment is made from embodiment 1.
After testing, the number of plies of graphene made from the present embodiment is about 3 layers.
Embodiment 3
The preparation method of graphene provided in this embodiment includes the following steps:
(1) 1g amorphous graphites powder is uniformly mixed into planetary with 3g sodium sulfites and grinds 150h, grinding is finished, obtained
Mix presoma；
(2) step (1) mixing presoma obtained is mixed with 350mL isopropanols, then sequentially adds 50g through mercapto
The poly-dopamine of base hydroxyethyl starch modification, 30g polyvinylpyrrolidones, after stirring evenly, are surpassed with ultrasonic generator
Sonication, ultrasonic time 1h, ultrasonic power 300W obtain graphite ene product then through washing, centrifugation, 50 DEG C of dryings；
The poly-dopamine modified through sulfhydrylation hydroxyethyl starch used in the present embodiment is made from embodiment 1.
After testing, the number of plies of graphene made from the present embodiment is about 3~4 layers.
Embodiment 4
The preparation method of graphene provided in this embodiment includes the following steps:
(1) 1g expanded graphites powder is uniformly mixed with 5g sodium carbonate and carries out high-energy ball milling 100h, grinding is finished, mixed
Presoma；
(2) step (1) mixing presoma obtained is mixed with 350mL ethyl alcohol, then sequentially adds 30g through sulfydryl
Poly-dopamine, the 50g polyvinylpyrrolidones for changing hydroxyethyl starch modification, after stirring evenly, ultrasound is carried out with ultrasonic generator
Processing, ultrasonic time 1h, ultrasonic power 300W obtain graphite ene product then through washing, centrifugation, 50 DEG C of dryings；
The poly-dopamine modified through sulfhydrylation hydroxyethyl starch used in the present embodiment is made from embodiment 1.
After testing, the number of plies of graphene made from the present embodiment is about 3~4 layers.
Experimental example
Conducting performance test is carried out to graphene made from embodiment 2~4, test method is as follows：Using the auspicious tech in Ningbo
The FT-300I resistivity testers of device Co., Ltd are separately added into the cavity body of mould that internal diameter is 10mm, a height of 25mm on 2g
Graphene made from embodiment 2~4 is stated, 3.5MPa is forced into, is pressed into the thin slice of a diameter of 10mm, measures its conductivity,
As a result as follows：
The electric conductivity of graphene made from 1 embodiment 2~4 of table
| Conductivity (s/m) | |
| Embodiment 2 | 2500 |
| Embodiment 3 | 2550 |
| Embodiment 4 | 2500 |
As shown in Table 1, the present invention, using mechanical lapping, is then added through sulfhydrylation first by graphite powder and intercalator mixing
The poly-dopamine and dispersant of hydroxyethyl starch modification are ultrasonically treated, and having for graphene made from adopting said method is excellent
Electric conductivity, conductivity is up to 2500s/m or more, and the number of plies of graphene obtained is relatively low, have preferable performance.
Obviously, the above embodiments are merely examples for clarifying the description, and does not limit the embodiments.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of variation or
It changes.There is no necessity and possibility to exhaust all the enbodiments.And it is extended from this it is obvious variation or
It changes still within the protection scope of the invention.
Claims (10)
1. a kind of preparation method of graphene, which is characterized in that include the following steps:
(1) graphite powder is uniformly mixed with intercalator, using mechanical lapping mode, obtains mixing presoma；
(2) step (1) mixing presoma obtained is mixed with organic solvent, is sequentially added through sulfhydrylation hydroxyethyl starch
The poly-dopamine of modification, dispersant after stirring evenly, are ultrasonically treated, obtain graphite ene product.
2. the preparation method of graphene according to claim 1, which is characterized in that described to be repaiied through sulfhydrylation hydroxyethyl starch
The preparation method of the poly-dopamine of decorations is as follows:
(1) by hydroxyethyl starch carboxylated under alkaline condition, hydroxyl then is obtained by the reaction with 2- (two sulphur of pyridine)-ethylamine hydrochloride
Hydroxyethyl starch -2- (two sulphur of pyridine)；
(2) hydroxyethyl starch -2- made from the step (1) (two sulphur of pyridine) sulfhydrylation is obtained into sulfhydrylation hydroxyethyl starch；
(3) sulfhydrylation hydroxyethyl starch made from the step (2) is mixed with poly-dopamine and is reacted under alkaline condition
To the poly-dopamine modified by sulfhydrylation hydroxyethyl starch.
3. the preparation method of graphene according to claim 2, which is characterized in that in the step (3),
The mass ratio of the sulfhydrylation hydroxyethyl starch and the poly-dopamine is 5:1；
The pH of the alkaline condition is 10, and the reaction time is 30h.
4. the preparation method of graphene according to claim 2, which is characterized in that in the step (1), ethoxy is formed sediment
Powder under alkaline condition carboxylated the specific steps are：Hydroxyethyl starch is dissolved in deionized water, sodium hydroxide is sequentially added
It is reacted with monoxone and at 100 DEG C.
5. the preparation method of graphene according to claim 1, which is characterized in that in the step (1),
The graphite powder is crystalline flake graphite, expanded graphite or amorphous graphite；
The intercalator is sodium carbonate, sodium bicarbonate or sodium sulfite.
6. the preparation method of graphene according to claim 5, which is characterized in that the graphite powder and the intercalator
Mass ratio is 1:(3~10).
7. the preparation method of graphene according to claim 1, which is characterized in that in the step (1),
The mechanical lapping mode is horizontal grinding, planetary grinding or high-energy ball milling, the time of the mechanical lapping mode are
50~150h.
8. the preparation method of graphene according to claim 1, which is characterized in that the graphite powder with it is described through sulfhydrylation
The poly-dopamine of hydroxyethyl starch modification, the mass ratio of the dispersant are 1:(10~50):(30~80).
9. the preparation method of graphene according to claim 1, which is characterized in that the dispersant is detergent alkylate sulphur
Sour sodium or polyvinylpyrrolidone；The organic solvent is methanol, ethyl alcohol or isopropanol.
10. a kind of graphene being prepared according to claim 1-9 any one of them preparation methods.
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Cited By (2)
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| CN110759336A (en) * | 2019-11-11 | 2020-02-07 | 董影影 | Preparation method of graphene and graphene |
| CN111628172A (en) * | 2020-05-12 | 2020-09-04 | 山东领军科技集团有限公司 | Production process of graphene-based battery conductive agent |
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| CN111628172A (en) * | 2020-05-12 | 2020-09-04 | 山东领军科技集团有限公司 | Production process of graphene-based battery conductive agent |
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