CN109233282A - A kind of carbon nano tube-doped heat-conducting silicone grease of computer heat transmission and preparation method thereof - Google Patents
A kind of carbon nano tube-doped heat-conducting silicone grease of computer heat transmission and preparation method thereof Download PDFInfo
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- CN109233282A CN109233282A CN201810843907.2A CN201810843907A CN109233282A CN 109233282 A CN109233282 A CN 109233282A CN 201810843907 A CN201810843907 A CN 201810843907A CN 109233282 A CN109233282 A CN 109233282A
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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
- C08K9/04—Ingredients treated with organic substances
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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
- C08K3/041—Carbon nanotubes
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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
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/17—Amines; Quaternary ammonium compounds
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- 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
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
The invention belongs to heat-conducting silicone grease technical fields, and in particular to a kind of carbon nano tube-doped heat-conducting silicone grease of computer heat transmission and preparation method thereof.To single-walled carbon nanotube, successively acidified formation carboxyl, thionyl chloride chloride and mercaptoaniline form amide to the present invention, finally prepare organically-modified carbon nanotube to sulfydryl sealing end through isoflurane chalcone diisocyanate；The organically-modified carbon nanotube that the present invention prepares greatly improves the heat dissipation performance of heat-conducting silicone grease as the filler of heat-conducting silicone grease, and thermal conductivity can reach 6.98 W/ (m.K).
Description
Technical field
The invention belongs to heat-conducting silicone grease technical fields, and in particular to a kind of carbon nano tube-doped thermal conductive silicon of computer heat transmission
Rouge and preparation method thereof.
Background technique
With the rapid development of computer technology, as the central processing unit (Central of computer system core
Processing unit, CPU) arithmetic speed be getting faster, calorific value also increases with it.If CPU heat dissipation is bad, temperature
Spend height, it is easy to computer be caused to occur the problems such as thermal starting, crash in the process of running.Therefore, it is provided for CPU good
Cooling system is one of the essential condition for guaranteeing computer normal work.
Heat-conducting silicone grease is the paste containing silicone oil, and different heat-conducting silicone greases has different heating conductions.Due to manufacture
The limitation of technique, even surface-to-surface contact very smooth between CPU and cooling fin is also inevitably present a fixed gap,
And the presence in gap will severely impact the heat dissipation effect of CPU.People are usually filled in these gaps with heat-conducting silicone grease, to protect
The good contact between CPU and cooling fin is demonstrate,proved, contact area is increased, is finally reached the purpose for improving heat transfer efficiency.Therefore, thermally conductive
The quality of silicone grease heat dissipation performance will have crucial influence to the heat dissipation of CPU.
Carbon nanotube has high thermal conductivity, and the room temperature thermal conductivity for the single-wall carbon tube (SWNT) that molecular dynamics simulation calculates is high
Up to 6600W/ (m.K), experimental test goes out the room temperature thermal conductivity of multi-walled carbon nanotube (MWNT) up to 3000W/ (m.K), so carbon is received
Mitron is used to improve the thermal conductivity of heat-conducting silicone grease usually as the additive of heat-conducting silicone grease；University Of Nanchang's Liu Junfeng et al. (material
Scientific and engineering journal, 2009,27 (2): 271-273, carbon nanotube/heat-conducting silicone grease composite material heating conduction) in it is right
Carbon nanotube is added in AS-610B heat-conducting silicone grease after being successively acidified, being esterified as additive, and thermal coefficient is by being modified
Preceding 0.385W/ (m.K) is increased to 0.725W/ (m.K)；North China Electric Power University Chen Chuan et al. (Chinese adhesive, 2017,26
(8): 42-47, the preparation of carbon nanotube/boron nitride heat-conducting silicone grease and its heating conduction research) oil, nothing based on methyl-silicone oil
Water-ethanol is dispersing agent, CNTs (multi-walled carbon nanotube)/BN (boron nitride) impurity is heat filling, and it is multiple to prepare CNTs/BN
Close heat-conducting silicone grease；The thermal conductivity that CNTs (multi-walled carbon nanotube) composite heat-conducting silicone grease afterwards is added is increased to by 0.6117W/ (m.K)
0.6994W/ (m.K), improves 14.3%.
Though at present there are many heat-conducting silicone grease of carbon nanotube preparation, thermal conductivity also it is more carbon nano tube-doped before modified
It improves, but the heat conductivity of heat conduction silicate finally prepared is still lower, is prepared so how to carry out modification to carbon nanotube
The heat-conducting silicone grease of high heat conductance is the important directions of current technical research.
Summary of the invention
The object of the present invention is to provide a kind of carbon nano tube-doped heat-conducting silicone grease of computer heat transmission of high heat conductance, this hairs
Bright to single-walled carbon nanotube, successively acidified formation carboxyl, thionyl chloride chloride and mercaptoaniline form amide, final to pass through
Isoflurane chalcone diisocyanate prepares organically-modified carbon nanotube to sulfydryl sealing end；The organically-modified carbon that the present invention prepares is received
Mitron greatly improves the heat dissipation performance of heat-conducting silicone grease as the filler of heat-conducting silicone grease, and thermal conductivity can reach 6.98W/ (m.K).
According to the first aspect of the invention, the present invention provides a kind of preparation method of organically-modified carbon nanotube, institutes
It states organically-modified carbon nanotube and introduces carboxyl, thionyl chloride and carboxyl on single-walled carbon nanotube by the concentrated sulfuric acid and concentrated nitric acid acidification
Reaction forms acyl chlorides, p-Mercaptoaniline and acyl chlorides and forms amide, is most prepared afterwards through isoflurane chalcone diisocyanate sealing end；
Preferably, the preparation method of organically-modified carbon nanotube specifically comprises the following steps:
1) by 20mg single-walled carbon nanotube be placed in the 25ml concentrated sulfuric acid and concentrated nitric acid mixed liquor (concentrated sulfuric acid/concentrated nitric acid=3:
1) ultrasonic back flow reaction 6-8h, is centrifuged at 3,000 rpm after being then cooled to room temperature in, be washed to filtrate at after neutrality at 90 DEG C
Under be dried under vacuum to constant weight and obtain carboxyl carbon nanotube；FT-IR(KBr):1730cm-1Carbonyl characteristic peak；In acid condition, exist
The surface of single-walled carbon nanotube introduces carboxyl；
2) 15mg carboxyl carbon nanotube is taken to be placed in 10ml SOCl2In, the reflux of 0.2g N,N-Dimethylformamide is then added dropwise
16-24h is reacted, room temperature is then cooled to, is centrifuged at 3,000 rpm, dries at 60 DEG C to constant weight and obtains acyl chlorides base carbon nanotube；This
Converting carboxylate groups in carboxyl carbon nanotube are acyl chlorides by step, introduce p-Mercaptoaniline to improve activity；
3) acyl chlorides base carbon nanotube 15mg, 3mg p-Mercaptoaniline is taken to be placed in 5ml toluene, then back flow reaction 6-8h drops
It warms to room temperature, is centrifuged at 3,000 rpm, constant weight is dried under vacuum at 70 DEG C and obtains amide base carbon nanotube；This step passes through to be formed
P-Mercaptoaniline is introduced on single-walled carbon nanotube by amido bond, and forms exposed sulfydryl；
4) it takes amide base carbon nanotube 100mg ultrasonic disperse in 10ml N,N-Dimethylformamide, 100mg is then added
Isoflurane chalcone diisocyanate, 50mg triethylamine react 12-24h under nitrogen atmosphere, after reaction at 3,000 rpm from
The heart, centrifugation object successively washed with methylene chloride and N,N-Dimethylformamide, be dried under vacuum at 60 DEG C constant weight obtain it is organically-modified
Carbon nanotube；This step blocks sulfydryl exposed in carbon nanotube, shape using isoflurane chalcone diisocyanate as end-capping reagent
At final organically-modified carbon nanotube；
According to another aspect of the present invention, and organic the present invention provides a kind of purposes of organically-modified carbon nanotube
Silicone oil is mixed for preparing heat-conducting silicone grease；
Preferably, organically-modified carbon nanotubes percentage is 50-90%wt in heat-conducting silicone grease；
Preferably, the organic silicone oil be dimethicone, epoxy modified polysiloxane, vinyl silicone oil, polymethylphenyl siloxane fluid or
Hydroxy silicon oil；
Preferably, the organic silicone oil is hydroxy silicon oil, and the hydroxy silicon oil hydroxy radical content is 7.2%wt, at 25 DEG C
Viscosity is 19.6mm2/s；
Preferably, the organic silicone oil is hydroxy silicon oil, the weight percent of organically-modified carbon nanotube in heat-conducting silicone grease
For 70-80%wt；
According to another aspect of the invention, the present invention provides a kind of preparation method of heat-conducting silicone grease, include the following steps:
It is uniform that organically-modified carbon nanotube is placed in ultrasonic disperse in methanol, amphoteric surfactant dodecylamino third is then added
Sour sodium and organic silicone oil the ultrasound 2-4h at 30-40 DEG C；It is cooled to 0-5 DEG C, ultrasound decompression is de- in the case where pressure is P=-0.09MPa
Except solvent methanol, it is warming up to 90 DEG C of vacuum drying 3-5h after purifying methanol and obtains heat-conducting silicone grease.System of the present invention in heat-conducting silicone grease
Influence heat conductivity of heat conduction silicate is easily gathered during standby in order to solve organically-modified carbon nanotube nanoparticle in heat-conducting silicone grease
The problem of, the present invention adds a small amount of amphoteric surfactant sodium dodecyl aminopropionitrile in system, and in preparation process
Middle to be solved organically-modified carbon nanotube by the way of solvent supersonic, low temperature ultrasonic decompression precipitation and be unevenly distributed, thermal conductivity is low
The problem of, the characteristic of carbon nanotube high heat conductance is utilized to greatest extent.
Preferably, the additional amount of the sodium dodecyl aminopropionitrile is the 0.2- of organically-modified carbon nanotubes
0.8%wt；
Compared with prior art, the present invention has the advantage that
1) present invention is by organically-modified prepare organically-modified carbon nanotube and can be used for preparing height to carbon nanotube
The heat-conducting silicone grease of thermal conductivity；
2) present invention adds sodium dodecyl aminopropionitrile during preparing heat-conducting silicone grease, and adopts during the preparation process
It solves organically-modified carbon nanotube with the mode of solvent supersonic, low temperature ultrasonic decompression precipitation to be unevenly distributed, improves thermal conductive silicon
The thermal conductivity of rouge.
Specific embodiment
In order to make the objectives, technical solutions and advantages of the present invention clearer, With reference to embodiment, to this
Invention is further described.It should be understood that these descriptions are merely illustrative, and it is not intended to limit the scope of the invention.
Thermal conductivity test: the present invention is tested not using heat flow method using the heat conduction coefficient tester of model DRL-III-P
The thermal conductivity of heat-conducting silicone grease, testing standard MIL-I-49456A are prepared with embodiment.
Single-walled carbon nanotube used in embodiment is from Beijing Deco Dao Jin Science and Technology Ltd., model CNT400, pipe
Diameter is 1-2nm, and length is 0.5-2 μm；The silicone oil that dimethicone is 50CS from the DOW CORNING trade name PMX-200 trade mark；
Epoxy modified polysiloxane is from Shandong Dayi Chemical Industry Co., Ltd, model DY-E701 epoxy modified polysiloxane, epoxide number
0.08mol/100g, viscosity are 1100cp (25 DEG C)；Vinyl silicone oil from pure prosperous chemical industry organosilicon material company of Shenzhen,
Viscosity is 2060mPa.S, contents of ethylene 1.1%wt；Polymethylphenyl siloxane fluid is from the pure prosperous chemical industry organosilicon material in Shenzhen
The BSO-30150 polymethylphenyl siloxane fluid of company；Hydroxy silicon oil is from pure prosperous chemical industry organosilicon material company of Shenzhen, hydroxy radical content
For 7.2%wt, the viscosity at 25 DEG C is 19.6mm2/ s, ring body content are 15.8%wt；Remaining reagent is commercially available in embodiment
Conventional reagent.
Embodiment 1
Organic modified carbon nano-tube is prepared by following process: 1, using the concentrated sulfuric acid and concentrated nitric acid acidification to single-walled carbon nanotube
It carries out acidification and introduces carboxyl；2, the carboxyl that acidification is formed is reacted to form acyl chlorides using thionyl chloride with carboxyl；3, using to mercapto
Base aniline and acyl chlorides form amide；4, sealing end formation is carried out to the sulfydryl in p-Mercaptoaniline using isoflurane chalcone diisocyanate
Final organically-modified carbon nanotube, it is specific the preparation method is as follows:
1) 20g single-walled carbon nanotube is placed in the mixed liquor (volume of the 200ml 98%wt concentrated sulfuric acid and 68%wt concentrated nitric acid
Than the concentrated sulfuric acid/concentrated nitric acid=3:1) in ultrasonic back flow reaction 6-8h, be centrifuged, wash at 3,000 rpm after being then cooled to room temperature
Carboxyl carbon nanotube is obtained at constant weight is dried under vacuum to after neutrality at 90 DEG C to filtrate；FT-IR (KBr pressed disc method): occur
1730cm-1Carbonyl characteristic peak, it was demonstrated that existing carboxyl in carbon nanotube；
2) 15g carboxyl carbon nanotube is taken to be placed in 100ml SOCl2In, the reflux of 0.2g N,N-Dimethylformamide is then added dropwise
16-24h is reacted, room temperature is cooled to, is centrifuged at 3,000 rpm, dries at 60 DEG C to constant weight and obtains acyl chlorides base carbon nanotube；
3) acyl chlorides base carbon nanotube 15g, 3g p-Mercaptoaniline is taken to be placed in 500ml toluene, then back flow reaction 6-8h drops
It warms to room temperature, is centrifuged at 3,000 rpm, constant weight is dried under vacuum at 70 DEG C and obtains amide base carbon nanotube；
4) it takes amide base carbon nanotube 100g ultrasonic disperse in 1L N,N-Dimethylformamide, the different fluorine of 100g is then added
That ketone diisocyanate, 5g triethylamine react 12-24h under nitrogen atmosphere, are centrifuged at 3,000 rpm after reaction, are centrifuged
Object is successively washed with 500ml methylene chloride and 500ml N,N-Dimethylformamide, and constant weight is dried under vacuum at 60 DEG C and obtains organic change
Property carbon nanotube.
Embodiment 2
Be added in dimethicone organically-modified carbon nanotube (loading of organically-modified carbon nanotube be 60%wt,
Dimethicone loading is 40%wt), after mixing with stainless steel colloid mill, dry 30min makes in 130 DEG C of baking oven
It is thickened, and then obtains heat-conducting silicone grease within ultrasound 1-2 days at 60-70 DEG C, testing its thermal conductivity is 3.69W/ (m.K).
Embodiment 3
The selection of organic silicone oil type: organically-modified carbon nanotube (organically-modified carbon nanotube is added in organic silicone oil
Loading be 60%wt, organic silicone oil loading be 40%wt), after mixing with stainless steel colloid mill, in 130 DEG C of baking
Dry 30min makes its thickening in case, then obtains heat-conducting silicone grease within ultrasound 1-2 days at 60-70 DEG C, tests different organic silicone oils
The thermal conductivity for preparing heat-conducting silicone grease is shown in Table 1:
The different organic silicone oils of table 1 prepare the thermal conductivity of heat-conducting silicone grease
Test result shows the more other types of heat conductivity of heat conduction silicate of hydroxy silicon oil and organically-modified carbon nanotube composition
Silicone oil is high, it may be possible to since the oxygen atom in hydroxy silicon oil preferably can form hydrogen bond with organically-modified carbon nanotube, increase
The compatibility of silicone oil and organically-modified carbon nanotube, so that the thermal conducting path of heat-conducting silicone grease improves.
Embodiment 4
When the type for determining organic silicone oil is hydroxy silicon oil, the present invention does the loading of organically-modified carbon nanotube
Research: organically-modified carbon nanotube is added in hydroxy silicon oil and (changes the filling of hydroxy silicon oil and organically-modified carbon nanotube
Amount), after mixing with stainless steel colloid mill, dry 30min makes its thickening in 130 DEG C of baking oven, then at 60-70 DEG C
It obtains heat-conducting silicone grease within ultrasonic 1-2 days, tests the thermal conductivity that different loading ratios prepare heat-conducting silicone grease and be shown in Table 2:
The influence of 2 hydroxy silicon oil of table and organically-modified carbon nano-tube filled ratio to thermal conductivity
Embodiment 5
When using colloid mill mixing hydroxy silicon oil and organically-modified carbon nanotube, it is found that organically-modified carbon nanotube is easily poly-
Collection enables heat-conducting silicone grease to facilitate and disperses in radiating surface to overcome the technical problem, and the present invention is attempted using ultrasound in solvent
Mixing, then the method for precipitation prepares heat-conducting silicone grease, the method is as follows:
It is uniform that organically-modified carbon nanotube 10.0g is placed in ultrasonic disperse in 200ml methanol, 0.05g both sexes are then added
Surfactant sodium dodecyl base alanine sodium and 2.5g hydroxy silicon oil the ultrasound 2-4h at 30-40 DEG C；It is cooled to 0-5 DEG C,
Pressure is ultrasonic removed under reduced pressure solvent methanol under P=-0.09MPa, and 90 DEG C of vacuum drying 3-5h are warming up to after purifying methanol and are obtained
Heat-conducting silicone grease.
In preparation process and its heat-conducting silicone grease prepared occurs without the clustering phenomena of obvious organically-modified carbon nanotube, inspection
Surveying the heat conductivity of heat conduction silicate prepared is 6.98W/ (mK), and this method ratio uses colloid mill good mixing effect.
Although embodiments of the present invention are described in detail, it should be understood that, without departing from of the invention
In the case where spirit and scope, embodiments of the present invention can be made with various changes, replacement and change.
Claims (9)
1. a kind of preparation method of organically-modified carbon nanotube, it is characterised in that: the organically-modified carbon nanotube is by the concentrated sulfuric acid
Introduce carboxyl on single-walled carbon nanotube with concentrated nitric acid acidification, thionyl chloride react with carboxyl to be formed acyl chlorides, p-Mercaptoaniline with
Acyl chlorides forms amide, is most prepared afterwards through isoflurane chalcone diisocyanate sealing end.
2. preparation method according to claim 1, characterized by the following steps:
1) single-walled carbon nanotube is placed in in the mixed liquor of the concentrated sulfuric acid and concentrated nitric acid ultrasonic back flow reaction, be then cooled to room temperature from
The heart is washed to filtrate into drying to constant weight after neutrality and obtains carboxyl carbon nanotube；
2) carboxyl carbon nanotube is taken to be placed in SOCl2In, N,N-Dimethylformamide back flow reaction is then added dropwise, reaction terminates cooling
To room temperature, centrifugation, drying to constant weight obtain acyl chlorides base carbon nanotube；
3) acyl chlorides base carbon nanotube, p-Mercaptoaniline is taken to be placed in toluene, back flow reaction is cooled to room temperature after reaction, from
The heart, drying to constant weight obtain amide base carbon nanotube；
4) it takes amide base carbon nanotube ultrasonic disperse in N,N-Dimethylformamide, isophorone diisocyanate is then added
Ester, triethylamine react under nitrogen atmosphere, are centrifuged after reaction, and centrifugation object successively uses methylene chloride and nitrogen nitrogen dimethyl formyl
Amine washing, drying to constant weight obtain organically-modified carbon nanotube.
3. a kind of purposes of any one of claim 1-2 organically-modified carbon nanotube, it is characterised in that: mixed with organic silicone oil
Conjunction is used to prepare heat-conducting silicone grease.
4. purposes according to claim 3, it is characterised in that: the weight percent of organically-modified carbon nanotube in heat-conducting silicone grease
Than for 50-90%wt.
5. purposes according to claim 4, it is characterised in that: the organic silicone oil is dimethicone, epoxy-modified silicon
Oil, vinyl silicone oil, polymethylphenyl siloxane fluid or hydroxy silicon oil.
6. purposes according to claim 5, it is characterised in that: the organic silicone oil is hydroxy silicon oil.
7. purposes according to claim 6, it is characterised in that: the weight percent of organically-modified carbon nanotube in heat-conducting silicone grease
Than for 70-80%wt.
8. a kind of preparation method of heat-conducting silicone grease described in claim 3, it is characterised in that: organically-modified carbon nanotube is placed in first
Ultrasonic disperse is uniform in alcohol, and amphoteric surfactant sodium dodecyl aminopropionitrile and organic silicone oil is then added at 30-40 DEG C
Lower ultrasound 2-4h；It is cooled to 0-5 DEG C, the ultrasonic removed under reduced pressure solvent methanol in the case where pressure is P=- 0.09MPa, after purifying methanol
It is warming up to 90 DEG C of vacuum drying 3-5h and obtains heat-conducting silicone grease.
9. preparation method according to claim 8, it is characterised in that: the additional amount of the sodium dodecyl aminopropionitrile is
The 0.2-0.8%wt of organically-modified carbon nanotubes.
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| CN111218115A (en) * | 2020-02-28 | 2020-06-02 | 中国电子科技集团公司第五十八研究所 | Preparation method of high-thermal-conductivity silicone sheet and high-thermal-conductivity silicone sheet |
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| CN113150385A (en) * | 2021-04-13 | 2021-07-23 | 中联重科股份有限公司 | Method for treating carbon nanotubes, polyurethane composition, polyurethane piston and preparation method thereof |
| CN113817452A (en) * | 2021-09-13 | 2021-12-21 | 北京科技大学 | Preparation method of carbon nitride modified carbon nanotube composite heat-conducting silicone grease |
| CN114539876A (en) * | 2022-03-01 | 2022-05-27 | 高尧 | Corrosion-resistant heat-dissipation protective coating and preparation method thereof |
| CN115651301A (en) * | 2022-11-15 | 2023-01-31 | 暨南大学 | Biaxially oriented polyolefin agricultural film |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111218115A (en) * | 2020-02-28 | 2020-06-02 | 中国电子科技集团公司第五十八研究所 | Preparation method of high-thermal-conductivity silicone sheet and high-thermal-conductivity silicone sheet |
| CN111876227A (en) * | 2020-08-05 | 2020-11-03 | 扬州工业职业技术学院 | Layered liquid crystal lubricant with cleaning and anti-creeping performances and preparation method thereof |
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| CN113817452B (en) * | 2021-09-13 | 2022-09-16 | 北京科技大学 | Preparation method of carbon nitride modified carbon nanotube composite heat-conducting silicone grease |
| CN114539876A (en) * | 2022-03-01 | 2022-05-27 | 高尧 | Corrosion-resistant heat-dissipation protective coating and preparation method thereof |
| CN115651301A (en) * | 2022-11-15 | 2023-01-31 | 暨南大学 | Biaxially oriented polyolefin agricultural film |
| CN115651301B (en) * | 2022-11-15 | 2024-03-26 | 暨南大学 | Biaxially oriented polyolefin agricultural film |
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