CN105154028B - A kind of three-dimensional grapheme nano-fluid and preparation method thereof - Google Patents
A kind of three-dimensional grapheme nano-fluid and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of three-dimensional grapheme nano-fluids and preparation method thereof, the nano-fluid by under alkaline condition through oxidizing modification three-dimensional grapheme and base fluid form, wherein, the base fluid is water, ethylene glycol or silicone oil, and the weight part ratio of three-dimensional grapheme and base fluid is 1:10000-100:10000.Preparation method be by three-dimensional grapheme under alkaline condition through it is oxidizing it is modified mixed with base fluid, ultrasonication or ultrasonic water bath 10-80min to get.The present invention is using the three-dimensional grapheme of porous structure as filler, the heating conduction of base fluid can be greatly improved in the case where a small amount of addition, it will not be decomposed by the material after oxidation modification under alkaline condition in 200 DEG CXia functional groups, with good dispersibility, it is less prone to the poly- problem of sinking of filler, highest can be stabilized 12 months or more, have fabulous stability.
Description
Technical field
The invention belongs to nano-fluid technical fields, and in particular to one kind has both high thermal conductivity using three-dimensional grapheme as filler
Performance and the nano-fluid of high stability and preparation method thereof.
Background technique
Nano-fluid is that particle stabilized be suspended in conventional fluid (water, ethylene glycol etc.) of metal or non pinetallic nano is formed
A kind of novel heat exchange working medium.Existing research shows that compared with conventional fluid, nano-fluid have higher thermal coefficient and
Excellent heat exchange property can be widely applied to the fields such as vehicle, aerospace, electronics, meet high-power engine, insulation is started
The high load capacity of the equipment such as machine, air-conditioning device, supercomputer conducts heat and cooling requirement.
Two-dimensional graphene has perfect two dimensional crystal structure, its lattice is the hexagon surrounded by six carbon atoms,
With a thickness of an atomic layer, thermal coefficient is up to 5300W/mK, is better than carbon nanotube and diamond, and existing research at present will
Nano-fluid is made as filler in two-dimensional graphene.However two-dimensional graphene does not reach ideal for the raising of base fluid performance
As a result, this may be due to the fact, that the dispersibility of one, graphene and the contradictory problems of thermal conductivity, graphene has height
The chemical stability of degree, structural integrity, therefore hydrophily is poor, the usual stability of nano-fluid prepared using water as base fluid is poor, is
The surfactant for improving its hydrophily and being added, will be greatly reduced the heating conduction of graphene.Two, graphene pleat easy to reunite
Wrinkle, severely impacts the performance of its performance.Since graphene has very high specific surface area, have between graphene sheet layer
Very high van der Waals interaction, this also has led to graphene and easily reunites and fold, the change of the arbitrary parameter of nano-fluid
Can all graphene be had an impact by changing such as temperature, concentration, enable it that reunion and fold occurs, so that the performance of fluid is affected,
Simultaneously because the reunion of graphene and the sedimentation meeting that causes so that fluid occur blocking microchannel etc. in application process it is serious
Problem.
Patent 200710032556.9 discloses a kind of preparation method of graphite series nano fluid, is during the preparation process
The dispersibility of material is improved using surfactant, and the presence of surfactant can generate the thermal stability of nano-fluid
It influences, generally starts to occur to 50 degree or more unstable.
Patent 201310548295.1 discloses a kind of preparation method of graphene nanofluid, is using nitric acid etc
Strong oxidizer two-dimensional graphene is aoxidized, the material performance that is oxidized is injured big, causes performance decline serious.
In addition, theoretically two-dimensional graphene along the thermal coefficient of face internal channel may be up to 5000Wm-1K-1, and along vertical
It is very low to direction, therefore the heat transfer of two-dimensional graphene nano-fluid is mainly based on the internal channel of face, therefore limits it
Application range.
Summary of the invention
In order to overcome the above-mentioned deficiencies of the prior art, the primary purpose of the present invention is that providing one kind has both high thermal conductivity
With the three-dimensional grapheme nano-fluid of high stability.
Another object of the present invention is to provide the preparation methods of above-mentioned three-dimensional grapheme nano-fluid.
The present invention is achieved through the following technical solutions:
A kind of three-dimensional grapheme nano-fluid, the nano-fluid are by under alkaline condition through oxidizing modification
Three-dimensional grapheme and base fluid composition, wherein the base fluid is water, ethylene glycol or silicone oil, the parts by weight of three-dimensional grapheme and base fluid
Than for 1:10000-100:10000.
In nano-fluid of the invention, the loading of three-dimensional grapheme is more, and the heating conduction of material is higher, however it is steady
Qualitative to decline with the increase of loading, in order to comprehensively consider the heating conduction and stability of material, the present invention preferably three
The weight part ratio for tieing up graphene and base fluid is 1:10000-10:10000.
Three-dimensional (3D) graphene of the present invention typically refers to two dimension (2D) the graphene assembly with 3D structure, is
The new type functional material of graphene chemical field in recent years.2D graphene film is integrated into the assembly with 3D structure can be with
Electricity, optics, machinery, chemistry and the catalysis characteristics of Effective Regulation graphene, therefore 3D grapheme material not only has graphene
Intrinsic physicochemical property, three-dimensional porous micro/nano structure also make it have both large specific surface area, high mechanical strength, electronics biography
Lead excellent ability and mass transfer quickly equal good characteristics.
Well known method can be used in the preparation method of three-dimensional grapheme of the present invention, such as template, hydro-thermal method, solvent
Thermal method etc..
Preferably, the specific surface area > 1800m of the three-dimensional grapheme2/ g, conductivity > 1000S/m, partial size 500-
2000nm。
Preferably, the oxidant is the persulfates such as potassium peroxydisulfate, ammonium persulfate, sodium peroxydisulfate, and oxidant adds
The weight part ratio for entering amount and three-dimensional grapheme is 1:10-1:100.
The preparation method of three-dimensional grapheme nano-fluid of the present invention, includes the following steps:
(1) modified three-dimensional graphite is prepared through oxidizing modification under alkaline condition in three-dimensional grapheme
Alkene;
(2) modified three-dimensional grapheme is mixed with base fluid, ultrasonication or ultrasonic water bath 10-80min obtain three-dimensional
Graphene nanofluid.
Preferably, preferred ultrasonication 10-80min in step (2), to guarantee that three-dimensional grapheme can be preferably dispersed in
In base fluid.
Preferably, step (1) specifically comprises the following steps:
A, oxidant is dissolved in water, stirred 10-20 minutes, addition three-dimensional grapheme, adjusting pH value of water solution to 11-13,
Stirring 20-40 minutes, obtains mixed liquor;
B, mixed liquor is placed in ultrasonic water bath after ultrasound 20-40 minutes, then is heated to reflux 6-12 under the conditions of 75-90 DEG C
Hour, obtain finely dispersed suspension;
C, liquid is removed by suction filtration under vacuum in suspension, with the mixed liquor pair of oxidant containing 3-5wt% and 2-3wt% hydrogen peroxide
Filtered filter cake is cleaned, then is washed with deionized water to neutrality, is dried in vacuo to get modified three-dimensional grapheme powder
End.
Preferably, in step b, the temperature of the ultrasound is 20-40 DEG C, and temperature is excessively high, and oxidant can decompose, to influence
Oxidation effectiveness.
Preferably, in step c, the vacuum drying temperature is 40-60 DEG C, and the time is 12-36 hours.
The present invention can control the pH value of the solution at 11-13, persulfuric acid by hydroxide such as potassium hydroxide, sodium hydroxides
Salt oxidizing agent decomposable generation ion radical SO soluble in water4 -, persulfate decomposes acceleration in acid medium, will affect it
Oxidation susceptibility, therefore guarantee oxidation effectiveness using alkaline environment to mitigate its decomposition.
Compared with prior art, the present invention having the following beneficial effects:
(1) present invention can greatly improve in the case where a small amount of addition using the three-dimensional grapheme of porous structure as filler
The heating conduction of base fluid may make base fluid in the case where the weight part ratio of three-dimensional grapheme and base fluid is 1:10000-10:10000
Thermal conductivity improves 5-40%.
(2) present invention uses under alkaline condition, is oxidant to three-dimensional using persulfates such as potassium peroxydisulfate, ammonium persulfates
Graphene carries out oxidation processes, injures small, modified 3 D graphene powder good hydrophilic property obtained to the material performance being oxidized,
The compatibility for improving porous three-dimensional grapheme material Yu polarity base fluid is avoided using surfactant etc. to thermal stability shadow
Loud defect will not be decomposed in 200 DEG CXia functional groups by the material after oxidation modification, ensure that the stability of fluid.
(3) present invention has good dispersibility using the nano-fluid that ultrasonication or ultrasonic water bath method technique obtain,
It is less prone to the poly- problem of sinking of filler, highest can be stabilized 12 months or more, have fabulous stability.
Specific embodiment
Further illustrate that the present invention, following embodiment are the specific embodiment party of the present invention below by specific embodiment
Formula, but embodiments of the present invention are not limited by following embodiments.
Three-dimensional grapheme used by following embodiment is prepared into using the preparation method in patent 201210455913.3
It arrives, specific surface area is about 2000m2/ g, conductivity > 1000S/m, partial size 500-2000nm.
Embodiment 1:
(1) oxidation of three-dimensional grapheme, specifically includes the following steps:
A, potassium persulfate oxidation agent is dissolved in water, stirred 15 minutes, three-dimensional grapheme is added, adjusted with potassium hydroxide water-soluble
Liquid pH value stirs 30 minutes to 12, obtains mixed liquor;
B, mixed liquor is placed in 30 DEG C of ultrasonic water baths after ultrasound 30 minutes, then is heated to reflux 8 hours under the conditions of 90 DEG C,
Obtain finely dispersed suspension;
C, liquid is removed by suction filtration under vacuum in suspension, with the mixing of the agent and 3wt% hydrogen peroxide of potassium persulfate oxidation containing 5wt%
Liquid cleans filtered filter cake, then is washed with deionized water to neutrality, and 50 DEG C are dried in vacuo 24 hours to get modified
Three-dimensional grapheme.
(2) preparation of nano-fluid:
Modified three-dimensional grapheme is mixed for 1 part with 10000 parts of deionized water, ultrasonication 10min is to get three-dimensional
Graphene nanofluid, performance are as shown in table 1.
Embodiment 2:
(1) oxidation of three-dimensional grapheme, specifically includes the following steps:
A, ammonium persulfate oxidizing agent is dissolved in water, stirred 10 minutes, three-dimensional grapheme is added, adjusted with sodium hydroxide water-soluble
Liquid pH value stirs 20 minutes to 13, obtains mixed liquor;
B, mixed liquor is placed in 40 DEG C of ultrasonic water baths ultrasound after twenty minutes, then under the conditions of 80 DEG C to be heated to reflux 10 small
When, obtain finely dispersed suspension;
C, liquid is removed by suction filtration under vacuum in suspension, with the mixing of ammonium persulfate oxidizing agent containing 5wt% and 3wt% hydrogen peroxide
Liquid cleans filtered filter cake, then is washed with deionized water to neutrality, and 60 DEG C are dried in vacuo 12 hours to get modified
Three-dimensional grapheme.
(2) preparation of nano-fluid:
Modified three-dimensional grapheme is mixed for 1 part with 10000 parts of deionized water, ultrasonication 10min is to get three-dimensional
Graphene nanofluid, performance are as shown in table 1.
Embodiment 3:
(1) oxidation of three-dimensional grapheme, specifically includes the following steps:
A, potassium persulfate oxidation agent is dissolved in water, stirred 20 minutes, three-dimensional grapheme is added, adjusted with potassium hydroxide water-soluble
Liquid pH value stirs 30 minutes to 11, obtains mixed liquor;
B, mixed liquor is placed in 25 DEG C of ultrasonic water baths ultrasound after forty minutes, then under the conditions of 75 DEG C to be heated to reflux 12 small
When, obtain finely dispersed suspension;
C, liquid is removed by suction filtration under vacuum in suspension, with the mixing of the agent and 3wt% hydrogen peroxide of potassium persulfate oxidation containing 5wt%
Liquid cleans filtered filter cake, then is washed with deionized water to neutrality, and 40 DEG C are dried in vacuo 24 hours to get modified
Three-dimensional grapheme.
(2) preparation of nano-fluid:
Modified three-dimensional grapheme is mixed for 7 parts with 10000 parts of deionized water, ultrasonication 50min is to get three-dimensional
Graphene nanofluid, performance are as shown in table 1.
Embodiment 4:
Oxidant selects ammonium persulfate, remaining with embodiment 1,
Modified three-dimensional grapheme is mixed for 7 parts with 10000 parts of deionized water, ultrasonication 50min is to get three-dimensional
Graphene nanofluid, performance are as shown in table 1.
Embodiment 5:
Oxidant selects potassium peroxydisulfate, remaining with embodiment 1,
Modified three-dimensional grapheme is mixed for 7 parts with 10000 parts of deionized water, ultrasonic water bath 50min is to get three-dimensional
Graphene nanofluid, performance are as shown in table 1.
Embodiment 6:
The oxidation step of three-dimensional grapheme with embodiment 1,
Modified three-dimensional grapheme is mixed for 10 parts with 10000 parts of deionized water, ultrasonication 40min is to get three
Graphene nanofluid is tieed up, performance is as shown in table 1.
Embodiment 7:
The oxidation step of three-dimensional grapheme with embodiment 1,
Modified three-dimensional grapheme is mixed for 20 parts with 10000 parts of deionized water, ultrasonication 20min is to get three
Graphene nanofluid is tieed up, performance is as shown in table 1.
Embodiment 8:
The oxidation step of three-dimensional grapheme with embodiment 1,
Modified three-dimensional grapheme is mixed for 1 part with 10000 parts of ethylene glycol, ultrasonication 30min is to get three-dimensional stone
Black alkene nano-fluid, performance are as shown in table 1.
Embodiment 9:
The oxidation step of three-dimensional grapheme with embodiment 1,
Modified three-dimensional grapheme is mixed for 7 parts with 10000 parts of ethylene glycol, ultrasonication 60min is to get three-dimensional stone
Black alkene nano-fluid, performance are as shown in table 1.
Embodiment 10:
The oxidation step of three-dimensional grapheme with embodiment 1,
Modified three-dimensional grapheme is mixed for 20 parts with 10000 parts of ethylene glycol, ultrasonication 70min is to get three-dimensional
Graphene nanofluid, performance are as shown in table 1.
Embodiment 11:
The oxidation step of three-dimensional grapheme with embodiment 1,
Modified three-dimensional grapheme is mixed for 50 parts with 10000 parts of ethylene glycol, ultrasonication 80min is to get three-dimensional
Graphene nanofluid, performance are as shown in table 1.
Each performance parameter of 1 embodiment 1-11 nano-fluid of table
The present invention is using the three-dimensional grapheme of porous structure as the nano-fluid of filler it can be seen from 1 result of table, on the one hand
The heating conduction that base fluid can be greatly improved can in the case where the weight part ratio of three-dimensional grapheme and base fluid is 1:10000-10:10000
So that the thermal conductivity of base fluid improves 5-40%, on the other hand there is good dispersibility, place for a long time as can be seen from the table real
After testing, fluid does not occur apparent sedimentation, and highest can be stabilized 12 months or more, has fabulous stability, energy
Enough guarantee stability in use.
Claims (9)
1. a kind of three-dimensional grapheme nano-fluid, which is characterized in that the nano-fluid is by under alkaline condition through oxidant
The three-dimensional grapheme and base fluid of oxidation modification form, wherein the base fluid is water, ethylene glycol or silicone oil, three-dimensional grapheme and base
The weight part ratio of liquid is 1:10000-100:10000;The oxidant is in potassium peroxydisulfate, ammonium persulfate or sodium peroxydisulfate
It is one or more of.
2. three-dimensional grapheme nano-fluid according to claim 1, which is characterized in that the three-dimensional grapheme and base fluid
Weight part ratio is 1:10000-10:10000.
3. three-dimensional grapheme nano-fluid according to claim 1 or 2, which is characterized in that the three-dimensional grapheme tool
There are porous structure, specific surface area > 1800m2/ g, conductivity > 1000S/m, partial size 500-2000nm.
4. three-dimensional grapheme nano-fluid according to claim 1 or 2, which is characterized in that the addition of the oxidant
The weight part ratio of amount and three-dimensional grapheme is 1:10-1:100.
5. the preparation method of three-dimensional grapheme nano-fluid according to claim 1-4, which is characterized in that including
Following steps:
(1) modified three-dimensional grapheme is prepared through oxidizing modification under alkaline condition in three-dimensional grapheme;
(2) modified three-dimensional grapheme is mixed with base fluid, ultrasonication or ultrasonic water bath 10-80min obtain three-dimensional graphite
Alkene nano-fluid.
6. the preparation method of three-dimensional grapheme nano-fluid according to claim 5, which is characterized in that the step of step (2)
Suddenly are as follows: mix modified three-dimensional grapheme with base fluid, ultrasonication 10-80min obtains three-dimensional grapheme nano-fluid.
7. the preparation method of three-dimensional grapheme nano-fluid according to claim 5, which is characterized in that step (1) is specific
Include the following steps:
A, oxidant is dissolved in water, stirred 10-20 minutes, three-dimensional grapheme is added, adjust pH value of water solution to 11-13, stirring
20-40 minutes, obtain mixed liquor;
B, mixed liquor is placed in ultrasonic water bath after ultrasound 20-40 minutes, then under the conditions of 75-90 DEG C to be heated to reflux 6-12 small
When, obtain finely dispersed suspension;
C, liquid is removed by suction filtration under vacuum in suspension, with the mixed liquor of oxidant containing 3-5wt% and 2-3wt% hydrogen peroxide to suction filtration
Filter cake afterwards is cleaned, then is washed with deionized water to neutrality, is dried in vacuo to get modified three-dimensional grapheme powder.
8. the preparation method of three-dimensional grapheme nano-fluid according to claim 7, which is characterized in that described in step b
The temperature of ultrasound is 20-40 DEG C.
9. the preparation method of three-dimensional grapheme nano-fluid according to claim 7, which is characterized in that described in step c
Vacuum drying temperature is 40-60 DEG C, and the time is 12-36 hours.
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CN105923623A (en) * | 2016-04-19 | 2016-09-07 | 广西大学 | Preparation method of graphene powder with three-dimensional hierarchical porous structure |
CN108165016A (en) * | 2018-01-19 | 2018-06-15 | 林荣铨 | A kind of preparation method of modified graphene heat-conducting silicone grease |
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CN108929660B (en) * | 2018-07-03 | 2020-11-13 | 广东工业大学 | Composition and method for preparing nanofluid by using same |
CN109021935A (en) * | 2018-09-12 | 2018-12-18 | 北京科技大学 | A kind of preparation method of perfluoro triethylamine base high thermal conductivity lubrication nano-fluid |
CN114574163A (en) * | 2020-12-01 | 2022-06-03 | 中融美誉有限公司 | Graphene phase-change energy-gathering dispersion liquid and preparation method thereof |
CN114772588A (en) * | 2022-03-14 | 2022-07-22 | 鞍钢集团北京研究院有限公司 | Method for modifying activated carbon material and application thereof |
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