CN106744900A - A kind of preparation method of polymolecularity Graphene - Google Patents
A kind of preparation method of polymolecularity Graphene Download PDFInfo
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- CN106744900A CN106744900A CN201710023196.XA CN201710023196A CN106744900A CN 106744900 A CN106744900 A CN 106744900A CN 201710023196 A CN201710023196 A CN 201710023196A CN 106744900 A CN106744900 A CN 106744900A
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- graphene
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- C01—INORGANIC CHEMISTRY
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- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
Abstract
The present invention relates to field of graphene, and in particular to a kind of preparation method of polymolecularity Graphene, comprise the following steps：(1) by graphene powder ultrasonic disperse to organic solvent aqueous systems, Graphene powder dispersion liquid is prepared；(2) take silane coupler to be added in Graphene powder dispersion liquid, ultrasonic disperse after stirring in water bath reaction obtains the graphene solution of silane coupler grafting；(3) graphene solution that silane coupler is grafted is fitted into ball milling in ball grinder, collected through the graphene solution after ball milling, be concentrated under reduced pressure, drying obtains modified graphene；(4) absolute ethyl alcohol is added in modified powder, ultrasonic disperse after stirring, last vacuum freeze drying, secure satisfactory grades scattered property Graphene, the present invention can effectively improve the compatibility and adhesion of Graphene and other organic matters, and obtained Graphene is easily soluble in various solvents, it is easy to be equably combined with organic or inorganic material, it is difficult to reunite with polymolecularity, in application process.
Description
Technical field
The present invention relates to field of graphene, and in particular to a kind of preparation method of polymolecularity Graphene.
Background technology
Come into the Graphene in the popular visual field suddenly because of the Nobel Prize, as a kind of new two-dimensional nano carbonaceous material,
Extensive concern and in-depth study are caused in scientific circles.Graphene is to be in single layer of carbon atom thickness, by carbon atom
A kind of new carbonaceous material of bi-dimensional cellular shape lattice structure arrangement, it is considered to be basic group of every other dimension carbonaceous material
Into unit, the fullerene of zero dimension is such as can be bundled into, be curled into one-dimensional CNT, be piled into graphite of three-dimensional etc..Graphene
It is with sp by carbon atom2The monatomic carbon-coating that hydridization is combined into, structure is highly stable, with excellent mechanical property, peculiar
Electrical properties and good thermal property.Graphene due to its unique structure and excellent physical and chemical performance, in polymer matrix
The multiple fields such as composite, energy storage material, photoelectric device, biological medicine have a wide range of applications, and have attracted both at home and abroad
The very big concern of scientific research circle.
But one is there are problems that in the application process of Graphene, i.e., in the dispersion process of Graphene, due to complete knot
The Graphene of structure is made up of the benzene hexatomic ring containing stable keys, and chemical stability is high, the inert state in surface, mutual with other media
Effect is weaker, and graphene film interlayer has very strong intermolecular force, causes lamella to be easily stacked and is difficult to point
Scatter and, it is difficult to be dissolved in solvent, it more difficult to be equably combined with other organic or inorganic materials.This is further to Graphene
Research and application cause great difficulty, thus improve graphene dispersion and its with the compatibility of various solvents and material into
It is extension Graphene application field problem demanding prompt solution.
The content of the invention
The invention provides a kind of preparation method of polymolecularity Graphene, Graphene and other organic matters can be effectively improved
Compatibility and adhesion, obtained Graphene is easily soluble in various solvents, it is easy to equably multiple with organic or inorganic material
Close, with polymolecularity, agglomeration is less prone in application process.
To realize object above, the present invention is achieved by the following technical programs：
A kind of preparation method of polymolecularity Graphene, comprises the following steps：
(1) it is 0.3~0.5% by mass concentration in graphene powder ultrasonic disperse to organic solvent-aqueous systems, is prepared
Graphene powder dispersion liquid；
(2) take silane coupler to add into Graphene powder dispersion liquid, be well mixed, water-bath controls 65~75 DEG C, stirs
Mix 8~16h of reaction, after 1~2h of ultrasonic disperse at 40~50 DEG C, obtain the graphene solution of silane coupler grafting；
(3) graphene solution that stainless steel abrading-ball, silane coupler are grafted is fitted into ball grinder, in 200~300r/
6~10h of ball milling under the conditions of min, collects the graphene solution being grafted through the silane coupler after ball milling, is concentrated under reduced pressure, and dries, and obtains
Modified graphene；
(4) 0.5~1 times of absolute ethyl alcohol of amount is added in modified powder, 30~60min is stirred, ultrasound 4 at 30~40 DEG C
~6h, carries out vacuum freeze drying afterwards, obtains final product polymolecularity Graphene.
Preferably, the organic solvent in the step (1) in organic solvent-aqueous systems is ethanol, ethylene glycol, acetone, two
One kind in NMF.
Preferably, organic solvent and the volume ratio of water are 20~40: 1 in organic solvent-aqueous systems in the step (1).
Preferably, the silane coupler in the step (2) be γ-methacryloxypropyl trimethoxy silane,
One kind in APTES.
Preferably, silane coupler and the mass ratio of Graphene are 1: 10~20 in the step (2).
Preferably, the vacuum freeze drying specific control parameter for the treatment of in the step (4) is：10~30Pa of vacuum,
Solidification point -35~-30 DEG C, 20~24h of drying time.
Preferably, the supersonic frequency in the step (2), (4) is 15KHz.
Preferably, the drying mode in the step (3) is vacuum drying.
Preferably, 0.8 times of absolute ethyl alcohol of amount is added in the step (4) in modified powder, 50min, 35 DEG C is stirred
Lower ultrasonic 5h.
Beneficial effects of the present invention are：
1st, the present invention is modified using silane coupler to the dispersiveness of Graphene, silane coupled in modifying process
Agent is fully modified graphenic surface, and multi-layer graphene is abundant after ultrasonic disperse, ball grinder ball milling in dispersion process
Peel off into few layer or single-layer graphene.The graphenic surface modified through silane coupler increased active group, can improve graphite
The compatibility and adhesion of alkene and other organic matters, are easily soluble in various solvents, and are easy to organic or inorganic material equably
It is compound.
2nd, the present invention will carry out freeze-drying by the modified powder addition ethanol after ball milling, modified after freezing
There is polymolecularity, application process is less prone to agglomeration between Graphene.
Specific embodiment
To make the purpose, technical scheme and advantage of the embodiment of the present invention clearer, below in conjunction with the embodiment of the present invention,
Technical scheme in the embodiment of the present invention is clearly and completely described.Based on embodiments of the invention, the common skill in this area
The every other embodiment that art personnel are obtained under the premise of creative work is not made, belongs to the model of present invention protection
Enclose.
Embodiment 1：
A kind of preparation method of polymolecularity Graphene, comprises the following steps：
(1) Graphene powder that mass concentration is 0.5% will in graphene powder ultrasonic disperse to ethanol-water system, be prepared
Dispersion liquid, wherein ethanol are 30: 1 with the volume ratio of water.
(2) take silane coupler γ-methacryloxypropyl trimethoxy silane and add to graphene powder and disperse
In liquid, be well mixed, water-bath control 70 DEG C, stirring reaction 12h, after ultrasonic disperse 2h at 50 DEG C, obtain silane coupler
The graphene solution of grafting；Wherein γ-methacryloxypropyl trimethoxy silane and the mass ratio of graphene powder is 1
∶15；
(3) graphene solution that stainless steel abrading-ball, silane coupler are grafted is fitted into ball grinder, in 300r/min conditions
Lower ball milling 8h, collects the graphene solution being grafted through the silane coupler after ball milling, is concentrated under reduced pressure, and vacuum drying obtains modified stone
Black alkene；
(4) 0.8 times of absolute ethyl alcohol of amount is added in modified powder, 50min is stirred, ultrasound 5h, is carried out afterwards at 40 DEG C
Vacuum freeze drying, obtains final product polymolecularity Graphene.
Vacuum freeze drying in above-mentioned steps (4) processes specific control parameter：Vacuum 30Pa, solidification point -35
DEG C, drying time 24h.
Supersonic frequency in above-mentioned steps (2), (4) is 15KHz.
Embodiment 2：
A kind of preparation method of polymolecularity Graphene, comprises the following steps：
(1) Graphene that mass concentration is 0.3% will in graphene powder ultrasonic disperse to ethylene glycol-aqueous systems, be prepared
Powder dispersion, wherein ethylene glycol are 40: 1 with the volume ratio of water；
(2) take in silane coupler APTES addition Graphene powder dispersion liquid, be well mixed,
Water-bath controls 75 DEG C, stirring reaction 16h, after ultrasonic disperse 1.5h at 40 DEG C, obtain the Graphene of silane coupler grafting
Solution；Wherein APTES and the mass ratio of Graphene is 1: 10；
(3) graphene solution that stainless steel abrading-ball, silane coupler are grafted is fitted into ball grinder, in 200r/min conditions
Lower ball milling 6h, collects the graphene solution being grafted through the silane coupler after ball milling, is concentrated under reduced pressure, and vacuum drying obtains modified stone
Black alkene；
(4) 0.5 times of absolute ethyl alcohol of amount is added in modified powder, 60min is stirred, ultrasound 6h, is carried out afterwards at 30 DEG C
Vacuum freeze drying, obtains final product polymolecularity Graphene.
Vacuum freeze drying in above-mentioned steps (4) processes specific control parameter：Vacuum 10Pa, solidification point -30
DEG C, drying time 20h.
Supersonic frequency in above-mentioned steps (2), (4) is 15KHz.
Embodiment 3：
A kind of preparation method of polymolecularity Graphene, comprises the following steps：
(1) Graphene powder that mass concentration is 0.4% will in graphene powder ultrasonic disperse to acetone-water system, be prepared
Dispersion liquid, wherein acetone are 20: 1 with the volume ratio of water.
(2) take silane coupler γ-methacryloxypropyl trimethoxy silane and add Graphene powder dispersion liquid
In, be well mixed, water-bath control 65 DEG C, stirring reaction 8h, after ultrasonic disperse 1h at 45 DEG C, obtain silane coupler grafting
Graphene solution, the wherein mass ratio of γ-methacryloxypropyl trimethoxy silane and Graphene is 1: 20；
(3) graphene solution that stainless steel abrading-ball, silane coupler are grafted is fitted into ball grinder, in 250r/min conditions
Lower ball milling 10h, collects the graphene solution being grafted through the silane coupler after ball milling, is concentrated under reduced pressure, and vacuum drying obtains modified stone
Black alkene；
(4) 1 times of absolute ethyl alcohol of amount is added in modified powder, 30min, ultrasound 4h at 35 DEG C is stirred, is carried out afterwards true
Vacuum freecing-dry, obtains final product polymolecularity Graphene.
Vacuum freeze drying in above-mentioned steps (4) processes specific control parameter：Vacuum 20Pa, solidification point -32
DEG C, drying time 24h.
Supersonic frequency in above-mentioned steps (2), (4) is 15KHz.
Embodiment 4：
A kind of preparation method of polymolecularity Graphene, comprises the following steps：
(1) it is 0.5% by mass concentration in graphene powder ultrasonic disperse to dimethylformamide-aqueous systems, is prepared
Graphene powder dispersion liquid, wherein dimethylformamide are 40: 1 with the volume ratio of water；
(2) take in silane coupler APTES addition Graphene powder dispersion liquid, be well mixed,
Water-bath controls 65 DEG C, stirring reaction 8h, after ultrasonic disperse 2h at 50 DEG C, the Graphene for obtaining silane coupler grafting is molten
Liquid, wherein APTES are 1: 10 with the mass ratio of Graphene；
(3) graphene solution that stainless steel abrading-ball, silane coupler are grafted is fitted into ball grinder, in 200r/min conditions
Lower ball milling 10h, collects the graphene solution being grafted through the silane coupler after ball milling, is concentrated under reduced pressure, and vacuum drying obtains modified stone
Black alkene；
(4) 1 times of absolute ethyl alcohol of amount is added in modified powder, 30min, ultrasound 6h at 30 DEG C is stirred, is carried out afterwards true
Vacuum freecing-dry, obtains final product polymolecularity Graphene.
Vacuum freeze drying in above-mentioned steps (4) processes specific control parameter：Vacuum 15Pa, solidification point -35
DEG C, drying time 20h.
Supersonic frequency in above-mentioned steps (2), (4) is 15KHz.
Embodiment 5：
A kind of preparation method of polymolecularity Graphene, comprises the following steps：
(1) Graphene powder that mass concentration is 0.3% will in graphene powder ultrasonic disperse to ethanol-water system, be prepared
Dispersion liquid, wherein ethanol are 20: 1 with the volume ratio of water；
(2) take silane coupler γ-methacryloxypropyl trimethoxy silane and add Graphene powder dispersion liquid
In, be well mixed, water-bath control 75 DEG C, stirring reaction 16h, after ultrasonic disperse 1h at 40 DEG C, obtain silane coupler and connect
The graphene solution of branch, wherein γ-methacryloxypropyl trimethoxy silane are 1: 20 with the mass ratio of Graphene；
(3) graphene solution that stainless steel abrading-ball, silane coupler are grafted is fitted into ball grinder, in 300r/min conditions
Lower ball milling 6h, collects the graphene solution being grafted through the silane coupler after ball milling, is concentrated under reduced pressure, and vacuum drying obtains modified stone
Black alkene；
(4) 0.5 times of absolute ethyl alcohol of amount is added in modified powder, 40min is stirred, ultrasound 4h, is carried out afterwards at 40 DEG C
Vacuum freeze drying, obtains final product polymolecularity Graphene.
Vacuum freeze drying in above-mentioned steps (4) processes specific control parameter：Vacuum 30Pa, solidification point -30
DEG C, drying time 24h.
Supersonic frequency in above-mentioned steps (2), (4) is 15KHz.
Embodiment 6：
A kind of preparation method of polymolecularity Graphene, comprises the following steps：
(1) Graphene powder that mass concentration is 0.35% will in graphene powder ultrasonic disperse to acetone-water system, be prepared
Dispersion liquid, wherein acetone are 25: 1 with the volume ratio of water；
(2) take in silane coupler APTES addition Graphene powder dispersion liquid, be well mixed,
Water-bath controls 75 DEG C, stirring reaction 10h, after ultrasonic disperse 1h at 48 DEG C, the Graphene for obtaining silane coupler grafting is molten
Liquid, wherein APTES are 1: 18 with the mass ratio of Graphene；
(3) graphene solution that stainless steel abrading-ball, silane coupler are grafted is fitted into ball grinder, in 280r/min conditions
Lower ball milling 7h, collects the graphene solution being grafted through the silane coupler after ball milling, is concentrated under reduced pressure, and vacuum drying obtains modified stone
Black alkene；
(4) 0.7 times of absolute ethyl alcohol of amount is added in modified powder, 45min is stirred, ultrasound 4h, is carried out afterwards at 40 DEG C
Vacuum freeze drying, obtains final product polymolecularity Graphene.
Vacuum freeze drying in above-mentioned steps (4) processes specific control parameter：Vacuum 20Pa, solidification point -30
DEG C, drying time 24h.
Supersonic frequency in above-mentioned steps (2), (4) is 15KHz.
The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although with reference to the foregoing embodiments
The present invention has been described in detail, it will be understood by those within the art that：It still can be to foregoing each implementation
Technical scheme described in example is modified, or carries out equivalent to which part technical characteristic；And these modification or
Replace, do not make the spirit and scope of the essence disengaging various embodiments of the present invention technical scheme of appropriate technical solution.
Claims (9)
1. a kind of preparation method of polymolecularity Graphene, it is characterised in that：Comprise the following steps：
(1) graphite that mass concentration is 0.3~0.5% will in graphene powder ultrasonic disperse to organic solvent-aqueous systems, be prepared
Alkene powder dispersion；
(2) take silane coupler to add into Graphene powder dispersion liquid, be well mixed, water-bath controls 65~75 DEG C, and stirring is anti-
Answer 8~16h, after 1~2h of ultrasonic disperse at 40~50 DEG C, obtain the graphene solution of silane coupler grafting；
(3) graphene solution that stainless steel abrading-ball, silane coupler are grafted is fitted into ball grinder, in 200~300r/min bars
6~10h of ball milling under part, collects the graphene solution being grafted through the silane coupler after ball milling, is concentrated under reduced pressure, and dries, and obtains modified
Graphene；
(4) 0.5~1 times of absolute ethyl alcohol of amount is added in modified powder, 30~60min is stirred, ultrasonic 4 at 30~40 DEG C~
6h, carries out vacuum freeze drying afterwards, obtains final product polymolecularity Graphene.
2. the preparation method of polymolecularity Graphene according to claim 1, it is characterised in that：Have in the step (1)
Organic solvent in machine solvent-water system is the one kind in ethanol, ethylene glycol, acetone, dimethylformamide.
3. the preparation method of polymolecularity Graphene according to claim 1, it is characterised in that：Have in the step (1)
Organic solvent and the volume ratio of water are 20~40: 1 in machine solvent-water system.
4. the preparation method of polymolecularity Graphene according to claim 1, it is characterised in that：In the step (2)
Silane coupler is the one kind in γ-methacryloxypropyl trimethoxy silane, APTES.
5. the preparation method of polymolecularity Graphene according to claim 1, it is characterised in that：Silicon in the step (2)
Alkane coupling agent is 1: 10~20 with the mass ratio of graphene powder.
6. the preparation method of polymolecularity Graphene according to claim 1, it is characterised in that：In the step (4)
Vacuum freeze drying processes specific control parameter：10~30Pa of vacuum, solidification point -35~-30 DEG C, drying time 20~
24h。
7. the preparation method of the polymolecularity Graphene according to claim any one of 1-6, it is characterised in that：The step
(2), the supersonic frequency in (4) is 15KHz.
8. the preparation method of the polymolecularity Graphene according to claim any one of 1-6, it is characterised in that：The step
(3) drying mode in is vacuum drying.
9. the preparation method of the polymolecularity Graphene according to the hot any one of claim 1-6, it is characterised in that：The step
Suddenly 0.8 times of absolute ethyl alcohol of amount is added in (4) in modified powder, 50min, ultrasound 5h at 35 DEG C is stirred.
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Cited By (11)
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| 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 |
| WO2018233285A1 (en) * | 2017-06-24 | 2018-12-27 | 华为技术有限公司 | Functionalized graphene and preparation method therefor, and polyorganosiloxane |
| CN109368619A (en) * | 2018-11-20 | 2019-02-22 | 美盈森集团股份有限公司 | A kind of modified graphene and its preparation method and application |
| CN109735193A (en) * | 2019-01-02 | 2019-05-10 | 上海利物盛纳米科技有限公司 | Resistance to long-acting heavy-duty aqueous epoxy zinc-enriched paint based on graphene and preparation method thereof |
| CN109943111A (en) * | 2019-03-25 | 2019-06-28 | 中铁建大桥工程局集团第四工程有限公司 | A kind of preparation method of graphene-based anti-corrosion reinforcing bar |
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| CN112479194A (en) * | 2020-12-28 | 2021-03-12 | 三峡大学 | Graphene composite particle preparation device and method |
| CN113184841A (en) * | 2021-05-19 | 2021-07-30 | 深圳港创建材股份有限公司 | Method for enhancing dispersibility of low-oxygen-content graphene |
| CN113980426A (en) * | 2021-10-21 | 2022-01-28 | 浙江工业大学 | Modified graphene toughened epoxy resin heat-resistant composite material and preparation method thereof |
| CN114539624A (en) * | 2022-03-07 | 2022-05-27 | 南京工业大学 | Modification method of high-dispersion amidated low-vitamin carbon material |
| CN114605840A (en) * | 2022-04-07 | 2022-06-10 | 深圳天元羲王材料科技有限公司 | Graphene naphthenic oil slurry and preparation method thereof |
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| WO2018233285A1 (en) * | 2017-06-24 | 2018-12-27 | 华为技术有限公司 | Functionalized graphene and preparation method therefor, and polyorganosiloxane |
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| CN113184841A (en) * | 2021-05-19 | 2021-07-30 | 深圳港创建材股份有限公司 | Method for enhancing dispersibility of low-oxygen-content graphene |
| CN113980426A (en) * | 2021-10-21 | 2022-01-28 | 浙江工业大学 | Modified graphene toughened epoxy resin heat-resistant composite material and preparation method thereof |
| CN114539624A (en) * | 2022-03-07 | 2022-05-27 | 南京工业大学 | Modification method of high-dispersion amidated low-vitamin carbon material |
| CN114605840A (en) * | 2022-04-07 | 2022-06-10 | 深圳天元羲王材料科技有限公司 | Graphene naphthenic oil slurry and preparation method thereof |
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| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| CB02 | Change of applicant information | ||
| CB02 | Change of applicant information |
Address after: 213002 Changzhou new North District Airport Industrial Park in Jiangsu Applicant after: Wahson Pipeline Technology Co Ltd Address before: 213002 Changzhou new North District Airport Industrial Park in Jiangsu Applicant before: Jiangsu Huasheng Plastic Co., Ltd. |
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| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20170531 |