CN109824045A - A kind of graphene dispersing solution and preparation method thereof of direct modified graphene preparation - Google Patents
A kind of graphene dispersing solution and preparation method thereof of direct modified graphene preparation Download PDFInfo
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- CN109824045A CN109824045A CN201910222592.4A CN201910222592A CN109824045A CN 109824045 A CN109824045 A CN 109824045A CN 201910222592 A CN201910222592 A CN 201910222592A CN 109824045 A CN109824045 A CN 109824045A
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- graphene
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- dispersing solution
- modified graphene
- dispersion liquid
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Abstract
The invention discloses a kind of graphene dispersing solutions and preparation method thereof of direct modified graphene preparation, graphene and modified material are mixed, mixed powder is added in deionized water later, and mixed solution is stirred, is ultrasonically treated, obtains the modified graphene dispersion liquid of stable dispersion.Modified graphene dispersion liquid production process of the present invention is simple, does not need expensive device, modified material price used is low, harmless.Modified graphene dispersing solution defect is few, graphene number of plies is thin, can meet to the higher industry requirement of graphene quality requirement.
Description
Technical field
The invention belongs to technical field of graphene, and in particular to a kind of graphene dispersing solution of direct modified graphene preparation
And preparation method thereof.
Background technique
Graphene is a kind of New Two Dimensional material, due to its unique two-dimensional hexagonal lattice structure, makes it while having
The superior characteristics such as high thermal conductivity, electric conductivity and superpower mechanical strength.From being found so far, graphene has become energy storage
The hot research of the various fields such as material, semiconductor material and anticorrosive paint.Graphene is due to its specific surface area height, layer and interlayer
There are Van der Waals forces, easily reunite.Most of application requirement graphene dispersions are in solution, but since graphene is largely reunited,
It is difficult to be dispersed into solution, to limit the practical application of graphene.
In the existing method of modifying for graphene aqueous dispersions, it is modified mostly for graphene oxide, so
After carry out reduction treatment, these method and steps are cumbersome, the device is complicated, and obtained redox graphene surface defect is big,
Reduced performance.
Summary of the invention
In view of the above-mentioned deficiencies in the prior art, the technical problem to be solved by the present invention is that providing a kind of direct modification
The graphene dispersing solution and preparation method thereof of graphene preparation, method and step is simple, and obtained graphene quality is high, and dispersion is steady
It is fixed.
The invention adopts the following technical scheme:
A kind of method that direct modified graphene prepares graphene dispersing solution, graphene and modified material is mixed to get mixed
Powder is closed, deionized water is then added into mixed-powder, pre-dispersed modified graphene dispersion liquid is made through magnetic agitation, so
Pre-dispersed modified graphene dispersion liquid is carried out afterwards to be ultrasonically treated the modified graphene dispersion liquid for being made stable.
Specifically, the mass ratio of graphene and modified material is 1:(1~20 in mixed-powder).
Further, modified material is neopelex, molecular formula C18H29NaO3S。
Specifically, graphene and the mass ratio of deionized water are 1:1000 in mixed-powder.
Specifically, the speed of magnetic agitation is 500~1000rpm.
Specifically, ultrasonic treatment is in two times, first time sonication treatment time is 15~45min, when being ultrasonically treated for the second time
Between be 1~2h.
Further, the power of ultrasonic treatment is 400~660W for the first time, the power of second ultrasonic treatment is 50~
120W。
Another technical solution of the invention is that a kind of modified graphene dispersion liquid, modified graphene dispersion liquid expands into
Big chip architecture, with a thickness of 2~3nm.
Compared with prior art, the present invention at least has the advantages that
The present invention is directly modified graphene, removes the reduction reaction of complex and difficult control, and preparation flow is simple,
Required equipment is simple, and technology difficulty reduces, and reduces production cost.
Further, since the present invention is directly modified graphene, in obtained graphene dispersing solution, graphene layer
Number is thin, defect is few, quality is high, and a kind of modified graphene dispersion liquid produced can meet higher to graphene quality requirement
Industry requirement.
Further, the present invention uses neopelex modified graphene, and the modified material price is low, to human body
Cost that is harmless, further reducing production and use.
Further, present invention optimizes ultrasonic techniques, pass through short time large power supersonic and long-time small-power ultrasound
Cooperation, both made graphene and modified material carried out sufficient contact and interaction, and also solved large power supersonic generation
The problem of a large amount of heat affecting graphene quality, while further reducing production cost.
Modified graphene dispersion phase prepared by the present invention is produced compared with the peak position at the peak 2D of unmodified graphene to lower wave number
Displacement is given birth to, the number of plies is thinned, and (002) peak peak position deviates to the left, and graphene layer spacing expands, and is dispersed more stable.
In conclusion the problems such as present invention efficiently solves the stable problem of graphene dispersing solution, production process is complicated, changes
Graphene dispersing solution defect after property is few, graphene number of plies is thin, can meet to the higher industry requirement of graphene quality requirement.
Below by drawings and examples, technical scheme of the present invention will be described in further detail.
Detailed description of the invention
Fig. 1 is macroscopical comparison diagram that the present invention prepares sample；
Fig. 2 is the atomic force microscope microscopic appearance figure that the present invention prepares sample；
Fig. 3 is the Raman spectrogram that the present invention prepares sample；
Fig. 4 is the X-ray diffractogram that the present invention prepares sample.
Specific embodiment
The present invention provides a kind of methods that direct modified graphene prepares graphene dispersing solution, using detergent alkylate sulphur
Sour sodium carries out non-covalent bond to graphene and is modified, and carries out ultrasound and obtain stable graphene dispersing solution.Prepared by this method
Graphene dispersing solution defect is few, the number of plies is thin, easy to operate.
A kind of method that direct modified graphene prepares graphene dispersing solution of the present invention, comprising the following steps:
S1, in mass ratio it is 1:(1~20) graphene and modified material are weighed, and mixed, obtain graphene mixing
Powder；
Modified material is neopelex, molecular formula C18H29NaO3S。
S2, according to graphene quality in graphene mixed-powder and deionized water quality than the ratio for 1:1000, by stone
Black alkene mixed-powder is added in deionized water, and is stirred using magnetic stirring apparatus, and magnetic stirring apparatus revolving speed is 500~
1000rpm obtains pre-dispersed modified graphene dispersion liquid；
S3, pre-dispersed modified graphene dispersion liquid is ultrasonically treated, ultrasonic treatment is divided into two processes, is respectively
High-power dispersion ultrasound and small-power stablize ultrasound, wherein high-power dispersion ultrasonic power is 400~660W, ultrasonic time 15
~45 minutes, it was 50~120W that small-power, which stablizes ultrasonic power, and ultrasonic time is 1~2 hour, obtained stable modified graphene
Dispersion liquid.
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention
In attached drawing, technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is
A part of the embodiment of the present invention, instead of all the embodiments.The present invention being described and shown in usually here in attached drawing is real
The component for applying example can be arranged and be designed by a variety of different configurations.Therefore, below to the present invention provided in the accompanying drawings
The detailed description of embodiment be not intended to limit the range of claimed invention, but be merely representative of of the invention selected
Embodiment.Based on the embodiments of the present invention, those of ordinary skill in the art are obtained without creative efforts
The every other embodiment obtained, shall fall within the protection scope of the present invention.
Embodiment 1
(1) 10mg graphene and 10mg neopelex are weighed with electronic balance, the weighed powder of institute is put into
In reagent bottle；
(2) 10ml deionized water is weighed with graduated cylinder, and poured into reagent bottle；
(3) deionized water is stirred using magnetic stirring apparatus, revolving speed is set as 500rpm, obtains pre-dispersed modification
Graphene dispersing solution.
(4) pre-dispersed modified graphene dispersion liquid is put into progress large power supersonic dispersion in ultrasonic cell disrupte instrument,
Ultrasonic power is 650W, time 30min, and reagent bottle is put into progress small-power ultrasonic disperse in supersonic cleaning machine later, is surpassed
Acoustical power is 100W, and time 60min obtains the graphene dispersing solution of stable dispersion；
(5) gained graphene dispersing solution is named as G-1S, and according to test request, prepares respective sample.
Embodiment 2
(1) 10mg graphene and 50mg neopelex are weighed with electronic balance, the weighed powder of institute is put into
In reagent bottle；
(2) 10ml deionized water is weighed with graduated cylinder, and poured into reagent bottle；
(3) deionized water is stirred using magnetic stirring apparatus, revolving speed is set as 700rpm, obtains pre-dispersed modification
Graphene dispersing solution.
(4) pre-dispersed modified graphene dispersion liquid is put into progress large power supersonic dispersion in ultrasonic cell disrupte instrument,
Ultrasonic power is 650W, time 30min, and reagent bottle is put into progress small-power ultrasonic disperse in supersonic cleaning machine later, is surpassed
Acoustical power is 100W, and time 60min obtains the graphene dispersing solution of stable dispersion；
(5) gained graphene dispersing solution is named as G-5S, and according to test request, prepares respective sample.
Embodiment 3
(1) 10mg graphene and 200mg neopelex are weighed with electronic balance, the weighed powder of institute is put into
In reagent bottle；
(2) 1000ml deionized water is weighed with graduated cylinder, and poured into reagent bottle；
(3) deionized water is stirred using magnetic stirring apparatus, revolving speed is set as 1000rpm, obtains pre-dispersed change
Property graphene dispersing solution.
(4) pre-dispersed modified graphene dispersion liquid is put into progress large power supersonic dispersion in ultrasonic cell disrupte instrument,
Ultrasonic power is 400W, time 45min, and reagent bottle is put into progress small-power ultrasonic disperse in supersonic cleaning machine later, is surpassed
Acoustical power is 50W, and time 120min obtains the graphene dispersing solution of stable dispersion；
(5) graphene dispersing solution is made.
Embodiment 4
(1) 10mg graphene and 120mg neopelex are weighed with electronic balance, the weighed powder of institute is put into
In reagent bottle；
(2) 1000ml deionized water is weighed with graduated cylinder, and poured into reagent bottle；
(3) deionized water is stirred using magnetic stirring apparatus, revolving speed is set as 500rpm, obtains pre-dispersed modification
Graphene dispersing solution.
(4) pre-dispersed modified graphene dispersion liquid is put into progress large power supersonic dispersion in ultrasonic cell disrupte instrument,
Ultrasonic power is 660W, time 15min, and reagent bottle is put into progress small-power ultrasonic disperse in supersonic cleaning machine later, is surpassed
Acoustical power is 120W, and time 60min obtains the graphene dispersing solution of stable dispersion；
(5) graphene dispersing solution is made.
Referring to Fig. 1, G sample is unmodified graphene sample, G-1S is sample prepared by embodiment 1, and G-5S is to implement
Sample prepared by example 2.Can be visible in detail, using the modified graphene of neopelex, in deionized water
Dispersion is more abundant, stablizes.
Referring to Fig. 2, G sample is unmodified graphene sample, G-1S sample is sample prepared by embodiment 1, and G-5S is
Sample drawing prepared by embodiment 2.Can as seen from the figure, unmodified graphene sample is agglomerated into tubulose, and thickness is about 5nm；G-
1S and G-5S sample is the big chip architecture of expansion, with a thickness of 2~3nm.
Referring to Fig. 3, G sample is unmodified graphene sample, G-1S sample is sample prepared by embodiment 1, and G-5S is
Sample drawing prepared by embodiment 2.2700cm can be located at from figure-1The peak type at the peak 2D of left-right position finds out, unmodified graphite
Alkene thickness is at 5 layers or so, and modified G-1S and G-5S thickness of sample is at 2~3 layers or so.The peak position at the peak 2D, hair are observed simultaneously
Existing modified graphene sample produces displacement to lower wave number compared to the peak position at the peak 2D of unmodified graphene, also demonstrates layer
Number is thinned.
Referring to Fig. 4, G sample is unmodified graphene sample, G-1S sample is sample prepared by embodiment one, and G-5S is
Sample drawing prepared by embodiment two.The peak position at (002) peak it can find out that modified graphene sample does not change compared to from figure
Property graphene, peak position deviates to the left, it was demonstrated that graphene layer spacing expands, and disperses more stable.
The above content is merely illustrative of the invention's technical idea, and this does not limit the scope of protection of the present invention, all to press
According to technical idea proposed by the present invention, any changes made on the basis of the technical scheme each falls within claims of the present invention
Protection scope within.
Claims (8)
1. a kind of method that direct modified graphene prepares graphene dispersing solution, which is characterized in that by graphene and modified material
It is mixed to get mixed-powder, deionized water is then added into mixed-powder, pre-dispersed modified graphene is made through magnetic agitation
Then dispersion liquid carries out pre-dispersed modified graphene dispersion liquid being ultrasonically treated the modified graphene dispersion liquid for being made stable.
2. the method that direct modified graphene according to claim 1 prepares graphene dispersing solution, which is characterized in that mixing
The mass ratio of graphene and modified material is 1:(1~20 in powder).
3. the method that direct modified graphene according to claim 1 or 2 prepares graphene dispersing solution, which is characterized in that
Modified material is neopelex, molecular formula C18H29NaO3S。
4. the method that direct modified graphene according to claim 1 prepares graphene dispersing solution, which is characterized in that mixing
Graphene and the mass ratio of deionized water are 1:1000 in powder.
5. the method that direct modified graphene according to claim 1 prepares graphene dispersing solution, which is characterized in that magnetic force
The speed of stirring is 500~1000rpm.
6. the method that direct modified graphene according to claim 1 prepares graphene dispersing solution, which is characterized in that ultrasound
In two times, first time sonication treatment time is 15~45min for processing, and second of sonication treatment time is 1~2h.
7. the method that direct modified graphene according to claim 6 prepares graphene dispersing solution, which is characterized in that first
The power of secondary ultrasonic treatment is 400~660W, and the power of second of ultrasonic treatment is 50~120W.
8. the modified graphene dispersion liquid that one kind is prepared method according to claim 1, which is characterized in that modified graphene point
Dispersion liquid expands into big chip architecture, with a thickness of 2~3nm.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104211053A (en) * | 2014-09-04 | 2014-12-17 | 济宁利特纳米技术有限责任公司 | Preparation method of modified graphene aqueous dispersion |
| CN108394892A (en) * | 2018-05-11 | 2018-08-14 | 西安交通大学 | A kind of graphene dispersion liquid and preparation method thereof that directly graphene is modified |
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- 2019-03-22 CN CN201910222592.4A patent/CN109824045A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104211053A (en) * | 2014-09-04 | 2014-12-17 | 济宁利特纳米技术有限责任公司 | Preparation method of modified graphene aqueous dispersion |
| CN108394892A (en) * | 2018-05-11 | 2018-08-14 | 西安交通大学 | A kind of graphene dispersion liquid and preparation method thereof that directly graphene is modified |
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Application publication date: 20190531 |