CN108165016A - A kind of preparation method of modified graphene heat-conducting silicone grease - Google Patents
A kind of preparation method of modified graphene heat-conducting silicone grease Download PDFInfo
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- CN108165016A CN108165016A CN201810054905.5A CN201810054905A CN108165016A CN 108165016 A CN108165016 A CN 108165016A CN 201810054905 A CN201810054905 A CN 201810054905A CN 108165016 A CN108165016 A CN 108165016A
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/02—Ingredients treated with inorganic substances
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/08—Materials not undergoing a change of physical state when used
- C09K5/14—Solid materials, e.g. powdery or granular
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
Abstract
The present invention relates to a kind of heat-conducting silicone greases more particularly to a kind of modified graphene heat-conducting silicone grease and preparation method thereof.The present invention uses graphene prepared by liquid phase ultrasound stripping method as raw material, it is handled by hydroxylating, so that the upper a certain number of hydroxyls of graphene edge connection, are added in heat-conducting silicone grease again by heat filling of modified graphene, modified graphene heat-conducting silicone grease are finally made later.By being modified to graphene, dispersibility of the graphene in heat-conducting silicone grease is improved, while also improve the compatibility of graphene and heat-conducting silicone grease.Modified graphene heat-conducting silicone grease produced by the present invention, stability, service life and heat conductivility are significantly improved.
Description
Technical field
The present invention relates to a kind of heat-conducting silicone greases more particularly to a kind of modified graphene heat-conducting silicone grease and preparation method thereof.
Background technology
Heat-conducting silicone grease (also known as thermal grease) is a kind of pasta hot interface Heat Conduction Material, available for fever or heat dissipation element
Heat dissipation has good heat conductivility, is commonly applied to the fields such as electronic product.It is mainly characterized by：Both fast quick-release had been can be applied to
Put the heat generated during electronic product use, can also be applied in the fields such as aerospace, electric to need to radiate, conduct heat or
The positions such as insulation；The amount of heat generated during electronic equipment use can be excluded in time, it is densification in electronic product, small-sized
Change, reliability, precision and service life etc. play an important roll.Heat-conducting silicone grease has good mobility, can fill
Above-mentioned gap so as to ensure that the close contact between electronic component and cooling fin, and increases contact area, improves heat transfer
Efficiency, and then generated heat quickly and evenly reaches cooling fin when can farthest heater element be worked, and makes to dissipate
Thermal effect reaches best.Therefore, the quality of heat-conducting silicone grease performance influences very big, art technology to the heat dissipation performance of electronic component
Personnel also have been devoted to the research better heat-conducting silicone grease of heat conductivility, to improve the heat conduction and heat radiation performance of product.
Graphene is with sp by single layer of carbon atom2The hexatomic ring planar structure that hydridization is formed, is a kind of Utopian two dimension
Planar materials.Due to its special two dimensional crystal structure, there are good mechanical strength, electron mobility, high-specific surface area etc.
Feature.Also there is very high theoretical thermal conductivity simultaneously, more than 5300W/mK, significantly larger than other carbon such as graphite, carbon nanotube
The thermal conductivity of material is the highest material of known thermal conductivity.Since graphene is isotropic in slice plane, in plane
There is no directionality for interior heat transfer.Therefore by graphene for heat conduction field, it is to have very much to develop novel heat conduction film
It necessity and most possibly realizes.
W.Yu et al. is had studied respectively with graphene microchip, redox graphene and graphene microchip/varigrained
Aluminium oxide is High thermal-conductive silicone grease prepared by heat filling, it is found that graphene microchip can greatly increase the thermal conductivity of basic fat
Energy.Since redox graphene porous structure is larger to the viscosity of silicone grease, it is only capable of increasing silicone grease under low concentration
Heat conductivility；Compared to single graphene microchip filler and alumina packing, graphene microchip/alumina composite filler has
Conduction effect is cooperateed with, the heat conductivility of silicone grease can be improved (referring to " YU W, XIE H, YIN L, et al.Exceptionally
high thermal conductivity of thermal grease：Synergistic effects of graphene
And alumina [J] .Int J Therm Sci, 2015,91：76-82. " and " YU W, XIE H, CHEN L, et
Al.Graphene based silicone thermal greases [J] .Phys Lett A, 2014,378 (3)：207-
211.”).Multi-layer graphene is added to leading for a kind of thermal conductivity 5.8W/ (mK) by K.M.Shahil et al.
In hot silicone grease, just basic fat heat conductivility can be greatly improved in a small amount of addition, and the thermal conductivity maximum after addition is up to 14W/ (mK)
(referring to " SHAHIL K M, BALANDIN A A.Graphene-multilayer graphene nanocomposites as
Highly efficient thermal interface materials [J] .Nano Lett, 2012,12 (2)：861-
867.”).A kind of heat conductive silicone grease composition is disclosed in the patent document for being CN102634212A in publication No., the heat-conducting silicone grease
Composition is mainly made of carbon nanotube, graphene, phase transformation capsule particle object and silicone oil etc..Can further it be added using carbon nanotube
The conduction of speed heat amount, and phase transformation capsule particle object is used to improve the initial temperature absorption rate in hot junction, finally in internal fluid shape
Into the composition being distributed by the full three-dimensional network that particle (phase transformation capsule)+line (carbon nanotube)+plane (graphene) etc. forms.
This heat conductive silicone grease composition has many characteristics, such as that thermal conductivity is high, thermal resistance value is low, so as to significantly improve the heat dissipation of heat-conducting silicone grease effect
Rate and service life have good practical value.
However, the graphene used in these researchs is loaded in heat-conducting silicone grease directly as heat filling, and thermal conductive silicon
Graphene in fat can reunite, and graphene is not uniformly dispersed in heat-conducting silicone grease, and the heat conduction for influencing heat-conducting silicone grease is equal
Even property.Meanwhile the compatibility between graphene and heat-conducting silicone grease is poor, this is also unfavorable for carrying for the heat conductivility of heat-conducting silicone grease
It rises.
Based on this, how by graphene uniform to be distributed in heat-conducting silicone grease, further improve the thermal conductivity of heat-conducting silicone grease
Can, it is that those skilled in the art need a great problem solved.
Invention content
For above-mentioned technical problem of the existing technology, the present invention provides a kind of preparation of modified graphene heat-conducting silicone grease
Method, the modified graphene in the heat conductive silica gel being prepared can be evenly distributed in heat conductive silica gel, and modified graphene is with leading
Compatibility between hot silicone grease greatly improves, and finally obtains the modified graphene heat-conducting silicone grease that heat conductivility significantly improves.Meanwhile
The present invention also provides the modified graphene powder of a kind of compatibility that can increase between modified graphene and heat-conducting silicone grease and dispersibility
The preparation method of body.
To achieve the above object, the present invention provides following technical scheme：
The present invention provides a kind of preparation method of modified graphene heat-conducting silicone grease, includes the following steps：
(1) it weighs a certain amount of graphene and is placed in 15~60min of ultrasonic disperse, magnetic in the NaOH solution of 10~20mol/L
The lower room temperature reaction 8 of power stirring~for 24 hours；
(2) start in reaction, 2~5mL, 30% H is slowly added dropwise after stirring 1h2O2Catalyst of the solution as reaction；
(3) solution reacted is filtered, removes lye, then filter cake is cleaned with deionized water, washed
To neutrality, then with deionized water ultrasonic disperse into modified graphene dispersion liquid；
(4) the modified graphene dispersion liquid prepared in step (3) is dried by the way of spray drying, is changed
Property graphene powder；
(5) modified graphene powder made from step (4) is placed in the vacuum drying oven under the conditions of 65~80 DEG C, vacuum is done
Dry 1~2h, to remove the residual moisture in modified graphene and be activated to modified graphene, the modification after being activated
Graphene powder；
(6) the blank heat-conducting silicone grease for weighing certain mass is placed in vacuum stirring kettle, and 1~2h is stirred under vacuum condition；
(7) weighing the modified graphene powder after activation obtained, adding proportion in certain mass ratio step (5) is
0.5~5%, it is placed in the blank heat-conducting silicone grease being stirred in step (6), and stir 1~2h under vacuum, makes modified stone
Black alkene powder and heat-conducting silicone grease are tentatively uniformly mixed；
(8) modified graphene heat-conducting silicone grease presoma tentatively uniformly mixed in step (7) is placed in constant-temperature vacuum baking oven
In, heating carries out maturation process to precursor；
(9) the modified graphene heat-conducting silicone grease presoma after maturation process in step (8) is placed in de-airing mixer
Persistently stir 12~48h, you can stirred evenly and the modified graphene heat-conducting silicone grease of stable dispersion.
Preferably, the present invention provides a kind of preparation method of modified graphene heat-conducting silicone grease, includes the following steps：
(1) 0.5~2g graphenes are weighed and are placed in 500mL, ultrasonic disperse 15 in the NaOH solution of 10~20mol/L~
60min, room temperature reaction 8 under magnetic agitation~for 24 hours；
(2) start in reaction, 2~5mL, 30% H is slowly added dropwise after stirring 1h2O2Catalyst of the solution as reaction, drop
Acceleration is 1~2 drop/s；
(3) using ultrafiltration membrane and millipore filter, the solution reacted is filtered, remove lye, then spend from
Sub- water cleans filter cake, is washed to neutral (pH is believed that when being 6.5~7.5 has been washed to neutrality), then spend from
Sub- water ultrasonic disperse is into the modified graphene dispersion liquid of 1~5g/L；
(4) the modified graphene dispersion liquid prepared in step (3) is dried by the way of spray drying, is changed
Property graphene powder；
(5) modified graphene powder made from step (4) is placed in the vacuum drying oven under the conditions of 65~80 DEG C, vacuum is done
Dry 1~2h, to remove the residual moisture in modified graphene and be activated to modified graphene, the modification after being activated
Graphene powder；
(6) the blank heat-conducting silicone grease for weighing certain mass is placed in vacuum stirring kettle, and 1~2h is stirred under vacuum condition,
Blender rotating speed is 400~600r/min, and vacuum degree is -0.1MPa；
(7) weighing the modified graphene powder after activation obtained, adding proportion in certain mass ratio step (5) is
0.5~5%, be placed in the blank heat-conducting silicone grease being stirred in step (6), and 200~400r/min rotating speeds and vacuum degree for-
Under the conditions of 0.1Mpa, 1~2h is stirred, modified graphene powder and heat-conducting silicone grease is made tentatively to be uniformly mixed；
(8) by modified graphene heat-conducting silicone grease presoma tentatively uniformly mixed in step (7) be placed in temperature for 120~
180 DEG C, vacuum degree is in the constant-temperature vacuum baking oven of -0.1Mpa, heats 1~2h, and maturation process is carried out to precursor；
(9) by the modified graphene heat-conducting silicone grease presoma after maturation process in step (8) be placed in vacuum degree for-
12~48h is persistently stirred with the rotating speed of 800~1500r/min in the de-airing mixer of 0.1Mpa, you can stirred evenly and
The modified graphene heat-conducting silicone grease of stable dispersion.
Preferably, heat-conducting silicone grease selects Kraft spy's K-5211 heat-conducting silicone greases, this is conducive to the thermal conductivity for improving heat-conducting silicone grease
Can, obtained modified graphene heat-conducting silicone grease can be applied to LED lamp bead and radiate with radiating fin or pedestal junction.
The present invention also provides a kind of modified graphene raw powder's production technologies, include the following steps：
(1) it weighs a certain amount of graphene and is placed in 15~60min of ultrasonic disperse, magnetic in the NaOH solution of 10~20mol/L
The lower room temperature reaction 8 of power stirring~for 24 hours；
(2) start in reaction, 2~5mL, 30% H is slowly added dropwise after stirring 1h2O2Catalyst of the solution as reaction；
(3) solution reacted is filtered, removes lye, then filter cake is cleaned with deionized water, washed
To neutrality, then with deionized water ultrasonic disperse into modified graphene dispersion liquid；
(4) the modified graphene dispersion liquid prepared in step (3) is dried by the way of spray drying, is changed
Property graphene powder；
(5) modified graphene powder made from step (4) is placed in the vacuum drying oven under the conditions of 65~80 DEG C, vacuum is done
Dry 1~2h, to remove the residual moisture in modified graphene and be activated to modified graphene, the modification after being activated
Graphene powder.
Preferably, a kind of modified graphene raw powder's production technology, includes the following steps：
(1) 0.5~2g graphenes are weighed and are placed in 500mL, ultrasonic disperse 15 in the NaOH solution of 10~20mol/L~
60min, room temperature reaction 8 under magnetic agitation~for 24 hours；
(2) start in reaction, 2~5mL, 30% H is slowly added dropwise after stirring 1h2O2Catalyst of the solution as reaction, drop
Acceleration is 1~2 drop/s；
(3) using ultrafiltration membrane and millipore filter, the solution reacted is filtered, remove lye, then spend from
Sub- water cleans filter cake, is washed to neutral (pH is believed that when being 6.5~7.5 has been washed to neutrality), then spend from
Sub- water ultrasonic disperse is into the modified graphene dispersion liquid of 1~5g/L；
(4) the modified graphene dispersion liquid prepared in step (3) is dried by the way of spray drying, is changed
Property graphene powder；
(5) modified graphene powder made from step (4) is placed in the vacuum drying oven under the conditions of 65~80 DEG C, vacuum is done
Dry 1~2h, to remove the residual moisture in modified graphene and be activated to modified graphene, the modification after being activated
Graphene powder.
The present invention uses graphene prepared by liquid phase ultrasound stripping method to be handled for raw material by hydroxylating so that graphene
The upper a certain number of hydroxyls of edge connection, by being modified to graphene, improve dispersion of the graphene in heat-conducting silicone grease
Property, avoid graphene that agglomeration occurs in heat-conducting silicone grease, while also improve the compatibility of graphene and heat-conducting silicone grease.It
It, will by way of vacuum stirring using Kraft spy's K-5211 heat-conducting silicone grease base-materials afterwards again using modified graphene as heat filling
Modified graphene powder is added and is uniformly dispersed into Kraft spy's K-5211 heat-conducting silicone greases, forms novel modified graphene heat conduction
Silicone grease further promotes the heat conductivility of heat-conducting silicone grease.
Beneficial effects of the present invention：
Modified graphene has been made using hydroxylating processing in the present invention, improves dispersibility of the graphene in heat-conducting silicone grease
And compatibility, the stability of heat-conducting silicone grease can be improved, reduces from oil content, improves service life.Meanwhile the present invention passes through addition
A small amount of modified graphene powder can increase substantially the heat conductivility of heat-conducting silicone grease, greatly improved heat-conducting silicone grease performance and
Value.In addition, in the present invention, the preparation process of modified graphene heat-conducting silicone grease is simple, can be in existing heat-conducting silicone grease finished product
On the basis of directly add, be conveniently operated, it is at low cost, have a vast market prospect.
Description of the drawings
Fig. 1 is modified graphene heat-conducting silicone grease prepared by embodiment one；
Fig. 2 is the heat conductivility comparison diagram of modified graphene heat-conducting silicone grease prepared by embodiment one and blank heat-conducting silicone grease.
Specific embodiment
Below in conjunction with specific embodiment and attached drawing, the present invention is described in detail.
Embodiment one：The present invention provides a kind of preparation method of modified graphene heat-conducting silicone grease, includes the following steps：
(1) 1g graphenes are weighed and are placed in 500mL, ultrasonic disperse 30min in the NaOH solution of 10mol/L, under magnetic agitation
React at room temperature 12h；
(2) start in reaction, 5mL, 30% H is slowly added dropwise after stirring 1h2O2Catalyst of the solution as reaction, is added dropwise
Speed is 1 drop/s；
(3) using ultrafiltration membrane and millipore filter, the solution reacted is filtered, removes lye.Then spend from
Sub- water cleans filter cake, is washed to neutral (pH is believed that when being 6.5~7.5 has been washed to neutrality), then spend from
Sub- water ultrasonic disperse is into the modified graphene dispersion liquid of 3g/L；
(4) the modified graphene dispersion liquid prepared in step (3) is dried by the way of spray drying, is changed
Property graphene powder；
(5) modified graphene powder made from step (4) is placed in the vacuum drying oven under the conditions of 75 DEG C, be dried in vacuo
1h, to remove the residual moisture in modified graphene and be activated to modified graphene, the modified graphite after being activated
Alkene powder；
(6) the blank heat-conducting silicone grease for weighing certain mass is placed in vacuum stirring kettle, and stir 1h under vacuum condition, is stirred
Machine rotating speed is 400r/min, and vacuum degree is -0.1MPa；
(7) weighing the modified graphene powder after activation obtained, adding proportion in certain mass ratio step (5) is
1.2%, it is placed in the blank heat-conducting silicone grease being stirred in step (6), and be -0.1Mpa items in 300r/min rotating speeds and vacuum degree
Under part, 2h is stirred, modified graphene powder and heat-conducting silicone grease is made tentatively to be uniformly mixed；
(8) it is 150 DEG C modified graphene heat-conducting silicone grease presoma tentatively uniformly mixed in step (7) to be placed in temperature,
Vacuum degree is in the constant-temperature vacuum baking oven of -0.1Mpa, heats 1h, and maturation process is carried out to precursor；
(9) by the modified graphene heat-conducting silicone grease presoma after maturation process in step (8) be placed in vacuum degree for-
It is persistently stirred for 24 hours with the rotating speed of 1000r/min in the de-airing mixer of 0.1Mpa, you can stirred evenly and stable dispersion
Modified graphene heat-conducting silicone grease.
By modified graphene heat-conducting silicone grease obtained using homemade LED light thermal conductivity test device to the modification stone for preparing
The thermal conductivity of black alkene heat-conducting silicone grease carries out preliminary assessment.Meanwhile send sample to Guangzhou special type bearing device and detect research institute, lead to
Cross the true thermal conductivity factor of heat-conducting silicone grease heat conductivity measuring device test modified graphene heat-conducting silicone grease.
One preparation-obtained modified graphene heat-conducting silicone grease photo of the present embodiment is as shown in Figure 1, as can be seen from the figure
The color and luster of the modified graphene heat-conducting silicone grease is uniform, low from oil content, i.e. modified graphene powder is uniformly dispersed in heat-conducting silicone grease.
Fig. 2 is the heat conductivility comparison diagram of modified graphene heat-conducting silicone grease prepared by embodiment one and blank heat-conducting silicone grease.It is shown in Fig. 2
Two kinds of heat-conducting silicone greases are in heat conductivility test device by heat conductivility difference obtained from test.It can from Fig. 2
Going out, addition modified graphene heat-conducting silicone grease can be substantially reduced the temperature difference between the two between LED heat source and cooling base,
Show preferable heat conduction or heat-sinking capability.
The thermal conductivity factor of 1 modified graphene heat-conducting silicone grease of table and blank heat-conducting silicone grease
| Sample | Test temperature (DEG C) | Thermal conductivity factor W/ (mk) |
| Blank heat-conducting silicone grease | 25 | 0.533 |
| Modified graphene heat-conducting silicone grease | 25 | 0.803 |
The thermal conductivity factor of modified graphene heat-conducting silicone grease and blank heat-conducting silicone grease is listed in table 1, it can be seen that blank is led
The thermal conductivity factor of hot silicone grease is 0.533W/ (mk), and prepared modified graphene heat-conducting silicone grease is 0.803W/ (mk),
50.56% is improved by adding only 1.2wt.% modified graphenes powder, the heat conductivility for allowing for blank heat-conducting silicone grease,
Heat conductivility is obviously improved, i.e. modified graphene heat-conducting silicone grease can be applied to LED lamp bead and be connect with radiating fin or pedestal
Place's heat dissipation.
Finally it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention rather than the present invention is protected
The limitation of range is protected, although being explained in detail with reference to preferred embodiment to the present invention, those of ordinary skill in the art should
Work as understanding, technical scheme of the present invention can be modified or replaced equivalently, without departing from the reality of technical solution of the present invention
Matter and range.
Claims (6)
1. a kind of modified graphene raw powder's production technology, includes the following steps：
（1）It weighs a certain amount of graphene and is placed in 15 ~ 60 min of ultrasonic disperse, magnetic force in the NaOH solution of 10 ~ 20 mol/L and stir
Mix 8 ~ 24 h of lower room temperature reaction；
（2）Start in reaction, 2 ~ 5 mL, 30% H are slowly added dropwise after stirring 1h2O2Catalyst of the solution as reaction；
（3）The solution reacted is filtered, lye is removed, then filter cake is cleaned with deionized water, in being washed to
Property, then with deionized water ultrasonic disperse into modified graphene dispersion liquid；
（4）To step by the way of spray drying（3）The modified graphene dispersion liquid of middle preparation is dried, and obtains modified stone
Black alkene powder；
（5）By step（4）Modified graphene powder obtained is placed in the vacuum drying oven under the conditions of 65 ~ 80 DEG C, and vacuum drying 1 ~
2h, to remove the residual moisture in modified graphene and be activated to modified graphene, the modified graphite after being activated
Alkene powder.
2. modified graphene raw powder's production technology as described in claim 1, it is characterised in that：Include the following steps：
（1）It weighs 0.5 ~ 2g graphenes and is placed in 500mL, 15 ~ 60 min of ultrasonic disperse in the NaOH solution of 10 ~ 20 mol/L, magnetic
8 ~ 24 h of the lower room temperature reaction of power stirring；
（2）Start in reaction, 2 ~ 5 mL, 30% H are slowly added dropwise after stirring 1h2O2Catalyst of the solution as reaction, is added dropwise speed
It spends for 1 ~ 2 drop/s；
（3）Using ultrafiltration membrane and millipore filter, the solution reacted is filtered, lye is removed, then uses deionized water
Filter cake is cleaned, is washed to neutrality, then with deionized water ultrasonic disperse into the modified graphene dispersion liquid of 1 ~ 5 g/L；
（4）To step by the way of spray drying（3）The modified graphene dispersion liquid of middle preparation is dried, and obtains modified stone
Black alkene powder；
（5）By step（4）Modified graphene powder obtained is placed in the vacuum drying oven under the conditions of 65 ~ 80 DEG C, and vacuum drying 1 ~
2h, to remove the residual moisture in modified graphene and be activated to modified graphene, the modified graphite after being activated
Alkene powder.
3. a kind of preparation method of modified graphene heat-conducting silicone grease, includes the following steps：
（1）It weighs a certain amount of graphene and is placed in 15 ~ 60 min of ultrasonic disperse, magnetic force in the NaOH solution of 10 ~ 20 mol/L and stir
Mix 8 ~ 24 h of lower room temperature reaction；
（2）Start in reaction, 2 ~ 5 mL, 30% H are slowly added dropwise after stirring 1h2O2Catalyst of the solution as reaction；
（3）The solution reacted is filtered, lye is removed, then filter cake is cleaned with deionized water, in being washed to
Property, then with deionized water ultrasonic disperse into modified graphene dispersion liquid；
（4）To step by the way of spray drying（3）The modified graphene dispersion liquid of middle preparation is dried, and obtains modified stone
Black alkene powder；
（5）By step（4）Modified graphene powder obtained is placed in the vacuum drying oven under the conditions of 65 ~ 80 DEG C, and vacuum drying 1 ~
2h, to remove the residual moisture in modified graphene and be activated to modified graphene, the modified graphite after being activated
Alkene powder；
（6）The blank heat-conducting silicone grease for weighing certain mass is placed in vacuum stirring kettle, and 1 ~ 2h is stirred under vacuum condition；
（7）Weigh certain mass ratio step（5）In modified graphene powder after activation obtained, adding proportion for 0.5 ~
5%, it is placed in step（6）In in the blank heat-conducting silicone grease that is stirred, and stir 1 ~ 2h under vacuum, make modified graphene powder
Body and heat-conducting silicone grease are tentatively uniformly mixed；
（8）By step（7）In tentatively uniformly mixed modified graphene heat-conducting silicone grease presoma be placed in constant-temperature vacuum baking oven, add
Heat carries out maturation process to precursor；
（9）By step（8）Modified graphene heat-conducting silicone grease presoma after middle maturation process, which is placed in de-airing mixer, to be continued
Stir 12 ~ 48h, you can stirred evenly and the modified graphene heat-conducting silicone grease of stable dispersion.
4. the preparation method of modified graphene heat-conducting silicone grease as claimed in claim 3, it is characterised in that：Include the following steps：
（1）It weighs 0.5 ~ 2g graphenes and is placed in 500mL, 15 ~ 60 min of ultrasonic disperse in the NaOH solution of 10 ~ 20 mol/L, magnetic
8 ~ 24 h of the lower room temperature reaction of power stirring；
（2）Start in reaction, 2 ~ 5 mL, 30% H are slowly added dropwise after stirring 1h2O2Catalyst of the solution as reaction, is added dropwise speed
It spends for 1 ~ 2 drop/s；
（3）Using ultrafiltration membrane and millipore filter, the solution reacted is filtered, lye is removed, then uses deionized water
Filter cake is cleaned, is washed to neutrality, then with deionized water ultrasonic disperse into the modified graphene dispersion liquid of 1 ~ 5 g/L；
（4）To step by the way of spray drying（3）The modified graphene dispersion liquid of middle preparation is dried, and obtains modified stone
Black alkene powder；
（5）By step（4）Modified graphene powder obtained is placed in the vacuum drying oven under the conditions of 65 ~ 80 DEG C, and vacuum drying 1 ~
2h, to remove the residual moisture in modified graphene and be activated to modified graphene, the modified graphite after being activated
Alkene powder；
（6）The blank heat-conducting silicone grease for weighing certain mass is placed in vacuum stirring kettle, and 1 ~ 2h, blender are stirred under vacuum condition
Rotating speed is 400 ~ 600r/min, and vacuum degree is -0.1MPa；
（7）Weigh certain mass ratio step（5）In modified graphene powder after activation obtained, adding proportion for 0.5 ~
5%, it is placed in step（6）In in the blank heat-conducting silicone grease that is stirred, and be -0.1Mpa in 200 ~ 400r/min rotating speeds and vacuum degree
Under the conditions of, 1 ~ 2h is stirred, modified graphene powder and heat-conducting silicone grease is made tentatively to be uniformly mixed；
（8）By step（7）In tentatively uniformly mixed modified graphene heat-conducting silicone grease presoma to be placed in temperature be 120 ~ 180 DEG C,
Vacuum degree is in the constant-temperature vacuum baking oven of -0.1Mpa, heats 1 ~ 2h, and maturation process is carried out to precursor；
（9）By step（8）It is -0.1Mpa's that modified graphene heat-conducting silicone grease presoma after middle maturation process, which is placed in vacuum degree,
In de-airing mixer 12 ~ 48h is persistently stirred with the rotating speed of 800 ~ 1500r/min, you can stirred evenly and stable dispersion
Modified graphene heat-conducting silicone grease.
5. the modified graphene prepared by the preparation method of modified graphene heat-conducting silicone grease according to claim 3 or 4 is led
Hot silicone grease.
6. a kind of heat-conducting silicone grease containing modified graphene powder, it is characterised in that：The modified graphene powder is according to right
It is required that the method described in 1 or 2 is prepared.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810054905.5A CN108165016A (en) | 2018-01-19 | 2018-01-19 | A kind of preparation method of modified graphene heat-conducting silicone grease |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810054905.5A CN108165016A (en) | 2018-01-19 | 2018-01-19 | A kind of preparation method of modified graphene heat-conducting silicone grease |
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| Publication Number | Publication Date |
|---|---|
| CN108165016A true CN108165016A (en) | 2018-06-15 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114560703A (en) * | 2022-03-25 | 2022-05-31 | 山东百川智能科技有限公司 | Process for sintering silicon carbide ceramic through gel casting reaction |
| CN117089217A (en) * | 2021-09-04 | 2023-11-21 | 高祥 | Preparation method of heat-conducting engineering plastic |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11263613A (en) * | 1998-03-13 | 1999-09-28 | Nichirin Co Ltd | Intercalation complex of oxidized graphite and electrically conductive high molecular compound and its production |
| CN103570010A (en) * | 2013-10-17 | 2014-02-12 | 河南科技大学 | Preparation method of graphene powder material |
| CN103756325A (en) * | 2014-01-16 | 2014-04-30 | 广东工业大学 | Low-filling-capacity and high-heat-conductivity graphene/silicone grease composite material and preparation method thereof |
| CN103910354A (en) * | 2014-03-25 | 2014-07-09 | 复旦大学 | Method for preparing graphene through large-scale aqueous phase |
| CN104445169A (en) * | 2014-12-03 | 2015-03-25 | 安徽百特新材料科技有限公司 | Method for preparing grapheme by means of aqueous phase cutting and stripping |
| CN104893296A (en) * | 2015-06-05 | 2015-09-09 | 哈尔滨工业大学 | Composite silicone grease with high thermal conductivity and preparation method thereof |
| CN105154028A (en) * | 2015-10-14 | 2015-12-16 | 广东工业大学 | Three-dimensional graphene nanofluid and preparation method thereof |
| CN105838077A (en) * | 2016-04-06 | 2016-08-10 | 深圳市欧普特工业材料有限公司 | Surface treatment method of graphene used for producing heat conducting silicon sheets |
-
2018
- 2018-01-19 CN CN201810054905.5A patent/CN108165016A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11263613A (en) * | 1998-03-13 | 1999-09-28 | Nichirin Co Ltd | Intercalation complex of oxidized graphite and electrically conductive high molecular compound and its production |
| CN103570010A (en) * | 2013-10-17 | 2014-02-12 | 河南科技大学 | Preparation method of graphene powder material |
| CN103756325A (en) * | 2014-01-16 | 2014-04-30 | 广东工业大学 | Low-filling-capacity and high-heat-conductivity graphene/silicone grease composite material and preparation method thereof |
| CN103910354A (en) * | 2014-03-25 | 2014-07-09 | 复旦大学 | Method for preparing graphene through large-scale aqueous phase |
| CN104445169A (en) * | 2014-12-03 | 2015-03-25 | 安徽百特新材料科技有限公司 | Method for preparing grapheme by means of aqueous phase cutting and stripping |
| CN104893296A (en) * | 2015-06-05 | 2015-09-09 | 哈尔滨工业大学 | Composite silicone grease with high thermal conductivity and preparation method thereof |
| CN105154028A (en) * | 2015-10-14 | 2015-12-16 | 广东工业大学 | Three-dimensional graphene nanofluid and preparation method thereof |
| CN105838077A (en) * | 2016-04-06 | 2016-08-10 | 深圳市欧普特工业材料有限公司 | Surface treatment method of graphene used for producing heat conducting silicon sheets |
Non-Patent Citations (1)
| Title |
|---|
| RAO KS ET AL.: "Role of Peroxide Ions in Formation of Graphene Nanosheets by Electrochemical Exfoliation of Graphite", 《SCIENTIFIC REPORTS》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117089217A (en) * | 2021-09-04 | 2023-11-21 | 高祥 | Preparation method of heat-conducting engineering plastic |
| CN114560703A (en) * | 2022-03-25 | 2022-05-31 | 山东百川智能科技有限公司 | Process for sintering silicon carbide ceramic through gel casting reaction |
| CN114560703B (en) * | 2022-03-25 | 2023-03-21 | 山东百川智能科技有限公司 | Process for sintering silicon carbide ceramic through gel casting reaction |
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