CN109368629A - A kind of graphene dispersion system and preparation method thereof - Google Patents

A kind of graphene dispersion system and preparation method thereof Download PDF

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Publication number
CN109368629A
CN109368629A CN201811466110.1A CN201811466110A CN109368629A CN 109368629 A CN109368629 A CN 109368629A CN 201811466110 A CN201811466110 A CN 201811466110A CN 109368629 A CN109368629 A CN 109368629A
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China
Prior art keywords
graphene
dispersion system
graphene dispersion
dispersing agent
mass fraction
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CN201811466110.1A
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Chinese (zh)
Inventor
吕旺燕
黄丰
聂铭
刘世念
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Guangdong Power Grid Co Ltd
Electric Power Research Institute of Guangdong Power Grid Co Ltd
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Guangdong Power Grid Co Ltd
Electric Power Research Institute of Guangdong Power Grid Co Ltd
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Priority to CN201811466110.1A priority Critical patent/CN109368629A/en
Publication of CN109368629A publication Critical patent/CN109368629A/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/15Nano-sized carbon materials
    • C01B32/182Graphene
    • C01B32/194After-treatment

Abstract

The present invention relates to technical field of macromolecules more particularly to a kind of graphene dispersion system and preparation method thereof.The present invention provides a kind of graphene dispersion systems, including dispersing agent and the graphene being dispersed in the dispersing agent;The dispersing agent includes anion active agent and/or nonionic agent.The present invention also provides a kind of preparation methods of graphene dispersion system, comprising: step 1: by graphene predrying;Step 2: configuration high quality score dispersing agent, the concentration of the high quality score dispersing agent are 0.1g/L;Step 3: the graphene being added in the high quality score dispersing agent and obtains mixed solution;Step 4: by the mixed solution ultrasonic disperse and standing.A kind of graphene dispersion system provided by the invention and preparation method thereof, for solving the technical issues of cannot improving the dispersion performance of graphene aqueous suspension by surfactant-modified in the prior art.

Description

A kind of graphene dispersion system and preparation method thereof
Technical field
The present invention relates to technical field of macromolecules more particularly to a kind of graphene dispersion system and preparation method thereof.
Background technique
Carbon atom in graphene is with sp2Hydridization form, and the covalent bond and other carbon atoms that are 120 ° with angle connect Connect the hexagon stratiform honeycomb to be formed.On the direction perpendicular to layer plane, each carbon atom there are one pz track, because This can form the big pi bond of delocalization through holostrome.The ligancy of each carbon atom is 3 in layer, and the bond distance between adjacent carbon atom is about For 0.142nm, the dilute thickness of mono-layer graphite only 0.35nm.In addition to special monoatomic layer structure, graphene also has various excellent Different performance:.Single-layer graphene has the high grade of transparency (about 97.7%), and specific surface area calculated value can reach 2630m2/ g, Possess excellent mechanical property, brilliant electric property simultaneously.Its forbidden bandwidth is almost nil, carrier mobility is high, good Thermal property.Furthermore graphene also has fractional quantum hall effect, quantum Hall ferromagnetism and zero carrier mass fraction The series of characteristics such as the minimum electron conductivity under the limit.In conclusion graphene is with numerous excellent performances and more Unique structure is a kind of ideal second phase material.But a defect of graphene is exactly its dispersibility in aqueous solution Poor, the single-layer graphene for being prepared on a large scale surfactant-free in aqueous solution is always the unsolved problem of material circle, by In the huge specific surface area of graphene and as non-polar species, so that it is difficult to enter into water with extremely strong hydrophobicity It property solution and is evenly dispersed in water.The surfactant modified graphene hydrophobic grouping of someone so that its have it is certain Wetability and hydrophily, or graphene suspension body is directly prepared, it is prepared into suspension preservation.Currently, for dispersing stone There are mainly three types of the dilute systems of ink: aqueous surfactant solution, organic solvent, super acid.Above-mentioned three kinds of system electric conductivity and it can make Therefore cyanide-free plating bath failure cannot improve point of graphene aqueous suspension by surfactant-modified in the prior art Scattered performance becomes those skilled in the art's technical problem urgently to be resolved.
Summary of the invention
The present invention provides a kind of graphene dispersion systems and preparation method thereof, cannot pass through in the prior art for solving The technical issues of surfactant-modified dispersion performance to improve graphene aqueous suspension.
The present invention provides a kind of graphene dispersion systems, including dispersing agent and are dispersed in the dispersing agent Graphene;
The dispersing agent includes anion active agent and/or nonionic agent.
Preferably, the anion active agent includes sodium sulfate of polyethenoxy ether of fatty alcohol, dodecyl sodium sulfate, 12 One of sodium alkyl benzene sulfonate and sodium lignin sulfonate are a variety of.
Preferably, the mass fraction of the lauryl sodium sulfate is 0.6~3%.
Preferably, the mass fraction of the neopelex is 0.8~3%.
Preferably, the mass fraction of the fatty alcohol-ether sodium sulfate is 0.8~3%.
Preferably, the nonionic agent include polyoxethylene octylphenyl phenol ether -10, Tween-20, Tween-80 and One of polyvinylpyrrolidone is a variety of.
Preferably, the mass fraction of polyoxethylene octylphenyl phenol ether -10 is 0.4~2%;The mass fraction of the TW-20 It is 0.8~3%;The mass fraction of the TW-80 is 1~3%;The mass fraction of the PVP is 1~3%.
The present invention also provides a kind of preparation method of graphene dispersion system, including the following steps:
Step 1: by graphene predrying;
Step 2: configuration high quality score dispersing agent, the concentration of the high quality score dispersing agent are 0.1g/L;
Step 3: the graphene being added in the high quality score dispersing agent and obtains mixed solution;
Step 4: by the mixed solution ultrasonic disperse and standing.
Preferably, the pre-dried time is 1h.
Preferably, the time of ultrasonic disperse described in step 4 is 15min.
Dispersion provided in an embodiment of the present invention and preparation method thereof, by having collaboration between different surfaces activating agent The characteristic of effect, improving surfactant properties and can reduce the application cost of surfactant, and reduce surface-active Destruction of the agent to ecological environment, polynary surfactant compound have realistic meaning.Some researches show that work as ionic surfactant When nonionic surface active agent being added in agent, cmc (critical micelle concentration value) can be decreased obviously, and surface tension can also decline, Surface-active increases.So can be obtained when by carrying out single, binary or Recompounded multielement to the surfactant after preliminary screening Better dispersion stabilization.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this Some embodiments of invention without any creative labor, may be used also for those of ordinary skill in the art To obtain other attached drawings according to these attached drawings.
Fig. 1 is single surfactant-dispersed absorbance schematic diagram provided by the invention;
Fig. 2 is the first wetability schematic diagram of single surfactant provided by the invention;
Fig. 3 is the second wetability schematic diagram of single surfactant provided by the invention.
Specific embodiment
The embodiment of the invention provides a kind of graphene dispersion systems and preparation method thereof, for solving in the prior art not The technical issues of dispersion performance of graphene aqueous suspension can be improved by surfactant-modified.
In order to make the invention's purpose, features and advantages of the invention more obvious and easy to understand, below in conjunction with the present invention Attached drawing in embodiment, technical scheme in the embodiment of the invention is clearly and completely described, it is clear that disclosed below Embodiment be only a part of the embodiment of the present invention, and not all embodiment.Based on the embodiments of the present invention, this field Those of ordinary skill's all other embodiment obtained without making creative work, belongs to protection of the present invention Range.
Embodiment 1
Dispersing agent will affect the electric conductivity of plating solution as a kind of additive, and the parameters such as viscosity influence plating solution performance.Therefore Need to control its amount, so that controlling the amount of dispersing agent while it plays a role, not only having saved cost but also having and is good Effect, wherein the results are shown in Table 1 for the initial screening of single surfactant, single surfactant-dispersed absorbance size is such as Shown in Fig. 1, wetability is as shown in Figures 2 and 3.From the figure, it can be seen that surfactant additive amount before percent 1, is inhaled The size of luminosity increases sharply with the increase of surfactant concentration, concentration reach percent 2 or it is higher when, extinction Angle value tends towards stability.This is because in a certain amount of graphene suspension, the position of the adsorbable surfactant of graphene surface It sets and is limited, therefore, when surfactant reaches a certain concentration, not can be further improved point of absorbance and graphene Property is dissipated, because graphene surface has reached saturation.The quality of wetability can be intuitively from Fig. 2 and Fig. 3.Here wetting Property refer to graphene due to huge specific surface area and it be apolar substance, water is difficult to make as polar solvent It is contained therein with obtaining graphene stable and uniform, as shown in Figure 2.Suitable surfactant can utilize its hydrophobic grouping and stone Black alkene combines, and the demonstration of other end hydrophilic radical is made it possible to smoothly enter in water outside, stable dispersion reaches profit Wet effect, as shown in Figure 3.
The initial screening result of the single surfactant of table 1
Embodiment 2
Due to having synergistic effect between different surfaces activating agent, in order to improve surfactant properties, it is living to reduce surface Property agent application cost, and reduce destruction of the surfactant to ecological environment, dual surfactant compounding has reality Meaning.Some researches show that, when nonionic surface active agent is added in ionic surfactant, cmc value can be decreased obviously, Surface tension can also decline, and surface-active increases.So by carrying out binary built to the surfactant after preliminary screening, Better dispersion stabilization is obtained, the results are shown in Table 2:
2 dual surfactant of table compounds result
According to the size of absorbance and Zeta potential value is referred to, performance preferably binary built combination is respectively as follows: AES+ TW80、AES+TW20、SDS+TW20、SDS+PVP、SDBS+TW20、SDBS+PVP、SDBS+OP10、SDBS+TW80。
Embodiment 3
The more excellent result that binary built is obtained is further combined to obtain Recompounded multielement surfactant, polynary multiple With orthogonal result as shown in table 3 to table 6, the orthogonal preferred result of polynary surfactant is as shown in table 7:
More than 3 yuan of surfactant compound results of table
More than 4 yuan of surfactant compound results of table
More than 5 yuan of surfactant compound results of table
More than 6 yuan of surfactant compound results of table
More than 7 yuan of surfactants of table preferably compound result
The Zeta potential that summary analysis 3 measures after the absorbance and dilution of graphene water slurry into table 7 As a result, obtaining dispersion part Experiment conclusion, result is preferably compounded are as follows: SDBS (0.6%)+TW20 (1.5%)+PVP (1%).
The above, the above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations;Although referring to before Stating embodiment, invention is explained in detail, those skilled in the art should understand that: it still can be to preceding Technical solution documented by each embodiment is stated to modify or equivalent replacement of some of the technical features;And these It modifies or replaces, the spirit and scope for technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution.

Claims (10)

1. a kind of graphene dispersion system, which is characterized in that including dispersing agent and the stone being dispersed in the dispersing agent Black alkene;
The dispersing agent includes anion active agent and/or nonionic agent.
2. a kind of graphene dispersion system according to claim 1, which is characterized in that the anion active agent includes rouge One of fat alcohol polyethenoxy ether sodium sulfate, dodecyl sodium sulfate, neopelex and sodium lignin sulfonate or It is a variety of.
3. a kind of graphene dispersion system according to claim 2, which is characterized in that the matter of the lauryl sodium sulfate Measuring score is 0.6~3%.
4. a kind of graphene dispersion system according to claim 2, which is characterized in that the neopelex Mass fraction is 0.8~3%.
5. a kind of graphene dispersion system according to claim 2, which is characterized in that the matter of the fatty alcohol-ether sodium sulfate Measuring score is 0.8~3%.
6. a kind of graphene dispersion system according to claim 1, which is characterized in that the nonionic agent includes One of polyoxethylene octylphenyl phenol ether -10, Tween-20, Tween-80 and polyvinylpyrrolidone are a variety of.
7. a kind of graphene dispersion system according to claim 6, which is characterized in that polyoxethylene octylphenyl phenol ether -10 Mass fraction be 0.4~2%;The mass fraction of the TW-20 is 0.8~3%;The mass fraction of the TW-80 be 1~ 3%;The mass fraction of the PVP is 1~3%.
8. a kind of preparation method of graphene dispersion system, which is characterized in that including the following steps:
Step 1: by graphene predrying;
Step 2: configuration high quality score dispersing agent, the concentration of the high quality score dispersing agent are 0.1g/L;
Step 3: the graphene being added in the high quality score dispersing agent and obtains mixed solution;
Step 4: by the mixed solution ultrasonic disperse and standing.
9. a kind of graphene dispersion system according to claim 4, which is characterized in that the pre-dried time is 1h.
10. a kind of graphene dispersion system according to claim 4, which is characterized in that ultrasonic disperse described in step 4 Time is 15min.
CN201811466110.1A 2018-12-03 2018-12-03 A kind of graphene dispersion system and preparation method thereof Pending CN109368629A (en)

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110498634A (en) * 2019-08-02 2019-11-26 广西科技大学 A kind of graphene aqueous dispersions, graphene concrete and preparation method thereof
CN113105791A (en) * 2021-04-02 2021-07-13 河北晨阳工贸集团有限公司 Graphene modified aqueous thick elastic coating and preparation method thereof
CN113265235A (en) * 2020-02-14 2021-08-17 中国石油天然气股份有限公司 Modified graphene oxide hybrid guar gum fracturing fluid system and preparation method thereof
CN113584538A (en) * 2021-06-16 2021-11-02 南京清鹿新材料科技有限公司 Graphene-nicotinic acid silver plating solution and preparation method thereof
WO2022206926A1 (en) * 2021-04-01 2022-10-06 浙江正泰电器股份有限公司 Composite dispersant, preparation method therefor, mixed electroplating solution, and preparation method therefor
WO2022206927A1 (en) * 2021-04-01 2022-10-06 浙江正泰电器股份有限公司 Compound dispersant and preparation method, and mixed electroplating solution and preparation method
WO2022206923A1 (en) * 2021-04-01 2022-10-06 浙江正泰电器股份有限公司 Compound dispersant and preparation method, and mixed electroplating solution and preparation method
CN115182022A (en) * 2021-04-01 2022-10-14 浙江正泰电器股份有限公司 Compound dispersant and preparation method thereof, and mixed electroplating solution and preparation method thereof
CN115182019A (en) * 2021-04-01 2022-10-14 浙江正泰电器股份有限公司 Compound dispersant and preparation method thereof, and mixed electroplating solution and preparation method thereof
CN115182020A (en) * 2021-04-01 2022-10-14 浙江正泰电器股份有限公司 Compound dispersant, preparation method thereof, mixed electroplating solution and preparation method thereof

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102464315A (en) * 2010-11-18 2012-05-23 海洋王照明科技股份有限公司 Preparation method of graphene
US20140225026A1 (en) * 2013-02-13 2014-08-14 Basf Se Polyamide composites containing graphene
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
CN104495826A (en) * 2014-12-25 2015-04-08 北京航空航天大学 Single-layer graphene dispersion liquid and preparation method thereof
CN106902701A (en) * 2015-12-21 2017-06-30 天津瑞赛可新材料科技有限公司 A kind of graphene dispersion agent
CN106903324A (en) * 2015-12-22 2017-06-30 湖南利德电子浆料股份有限公司 A kind of preparation method of Graphene-nano silver dispersion
CN108250821A (en) * 2018-01-11 2018-07-06 绍兴文理学院 Graphene dispersion method for graphene-based anticorrosive paint
CN108486863A (en) * 2018-04-24 2018-09-04 济南圣泉集团股份有限公司 A kind of grapheme material modified fabric of antistatic and preparation method thereof

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102464315A (en) * 2010-11-18 2012-05-23 海洋王照明科技股份有限公司 Preparation method of graphene
US20140225026A1 (en) * 2013-02-13 2014-08-14 Basf Se Polyamide composites containing graphene
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
CN104495826A (en) * 2014-12-25 2015-04-08 北京航空航天大学 Single-layer graphene dispersion liquid and preparation method thereof
CN106902701A (en) * 2015-12-21 2017-06-30 天津瑞赛可新材料科技有限公司 A kind of graphene dispersion agent
CN106903324A (en) * 2015-12-22 2017-06-30 湖南利德电子浆料股份有限公司 A kind of preparation method of Graphene-nano silver dispersion
CN108250821A (en) * 2018-01-11 2018-07-06 绍兴文理学院 Graphene dispersion method for graphene-based anticorrosive paint
CN108486863A (en) * 2018-04-24 2018-09-04 济南圣泉集团股份有限公司 A kind of grapheme material modified fabric of antistatic and preparation method thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
侯海云: "《表面活性剂物理化学基础》", 31 August 2014, 西安交通大学出版社 *
张幼珠等: "《纺织应用化学》", 31 August 2009, 东华大学出版社 *

Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110498634A (en) * 2019-08-02 2019-11-26 广西科技大学 A kind of graphene aqueous dispersions, graphene concrete and preparation method thereof
CN113265235A (en) * 2020-02-14 2021-08-17 中国石油天然气股份有限公司 Modified graphene oxide hybrid guar gum fracturing fluid system and preparation method thereof
CN115182020A (en) * 2021-04-01 2022-10-14 浙江正泰电器股份有限公司 Compound dispersant, preparation method thereof, mixed electroplating solution and preparation method thereof
WO2022206926A1 (en) * 2021-04-01 2022-10-06 浙江正泰电器股份有限公司 Composite dispersant, preparation method therefor, mixed electroplating solution, and preparation method therefor
WO2022206927A1 (en) * 2021-04-01 2022-10-06 浙江正泰电器股份有限公司 Compound dispersant and preparation method, and mixed electroplating solution and preparation method
WO2022206923A1 (en) * 2021-04-01 2022-10-06 浙江正泰电器股份有限公司 Compound dispersant and preparation method, and mixed electroplating solution and preparation method
CN115182022A (en) * 2021-04-01 2022-10-14 浙江正泰电器股份有限公司 Compound dispersant and preparation method thereof, and mixed electroplating solution and preparation method thereof
CN115182019A (en) * 2021-04-01 2022-10-14 浙江正泰电器股份有限公司 Compound dispersant and preparation method thereof, and mixed electroplating solution and preparation method thereof
CN115182023A (en) * 2021-04-01 2022-10-14 浙江正泰电器股份有限公司 Compound dispersant, preparation method thereof, mixed electroplating solution and preparation method thereof
CN115182018A (en) * 2021-04-01 2022-10-14 浙江正泰电器股份有限公司 Compound dispersant and preparation method thereof, and mixed electroplating solution and preparation method thereof
CN115182017A (en) * 2021-04-01 2022-10-14 浙江正泰电器股份有限公司 Compound dispersant and preparation method thereof, and mixed electroplating solution and preparation method thereof
CN113105791A (en) * 2021-04-02 2021-07-13 河北晨阳工贸集团有限公司 Graphene modified aqueous thick elastic coating and preparation method thereof
CN113584538A (en) * 2021-06-16 2021-11-02 南京清鹿新材料科技有限公司 Graphene-nicotinic acid silver plating solution and preparation method thereof
CN113584538B (en) * 2021-06-16 2023-03-14 南京清鹿新材料科技有限公司 Graphene-nicotinic acid silver plating solution and preparation method thereof

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