CN108410178A - A kind of preparation method of the high thermal conductive silicon rubber of nitrogen aluminium/graphene hybrid material - Google Patents
A kind of preparation method of the high thermal conductive silicon rubber of nitrogen aluminium/graphene hybrid material Download PDFInfo
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- CN108410178A CN108410178A CN201810342321.8A CN201810342321A CN108410178A CN 108410178 A CN108410178 A CN 108410178A CN 201810342321 A CN201810342321 A CN 201810342321A CN 108410178 A CN108410178 A CN 108410178A
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- C—CHEMISTRY; METALLURGY
- 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
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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
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/28—Nitrogen-containing compounds
- C08K2003/282—Binary compounds of nitrogen with aluminium
Abstract
The invention discloses a kind of preparation methods of the high thermal conductive silicon rubber of nitrogen aluminium/graphene hybrid material, belong to the preparing technical field of high performance polymer material.The preparation method includes following procedure：(1) under the action of ultrasound, modified aluminium nitride and modified graphene are reacted, and nitride aluminum/graphite alkene hybrid material is prepared；(2) hybrid material, softening agent and anti-aging agent prepared by step (1) are added sequentially in silicon rubber, are kneaded using open mill, prepare rubber compound；(3) rubber compound for preparing step (2) it is thin it is logical for several times, it is thin it is logical during be added crosslinking agent, prepare vulcanizate, the high thermal conductive silicon rubber of as described nitrogen aluminium/graphene hybrid material through vulcanization after thin pass-out piece.Silicon rubber prepared by the present invention has good toughness and elasticity, excellent thermal conductivity, it is widely used in fixation in the fields such as heating, electrical, electronics, aviation between power device and radiator, antidetonation filling and Nian Jie, with significant economic value and social benefit.
Description
Technical field
The invention belongs to the preparing technical fields of high performance polymer material, and in particular to a kind of nitrogen aluminium/graphene
The preparation method of the high thermal conductive silicon rubber of hybrid material.
Technical background
Heat Conduction Material is widely used in the position for needing to radiate and conduct heat in Aeronautics and Astronautics, electronics and electric field.With
The progress of industrial expansion and science and technology, more stringent requirements are proposed to Heat Conduction Material by people, has both wished that it is carried for electronic component
For safe and reliable sinking path, and damping can be played the role of.Heat-conducting silicon rubber has special advantage in this respect, it was both
With high resiliency and heat resistance, and there is certain thermal conductivity.But the thermal coefficient of unmodified silicon rubber generally only has
0.165W/ (mK), therefore people are typically employed in silicon rubber and add Heat Conduction Material, as graphene, aluminium oxide, aluminium nitride,
Boron nitride etc. improves its thermal conductivity.(history wisdom, Li Ying, Yan Lu, the Cao Yunzhen such as history wisdom；Journal of Inorganic Materials, 2017,32
(9)：955-960) using with excellent heat conductivity graphene as filler, after graphene dispersing solution is freeze-dried with silver powder
It is jointly added in silicon rubber, prepares heat-conducting silicon rubber.When the volume content of graphene is 3%, the thermal coefficient of silicon rubber
4.900W/ (mK) when by being not added with graphene is increased to 12.367W/ (mK).Silver powder and graphene in this method
Dosage is larger, and cost is too high, can not large-scale industrial production.In recent years, in order to improve the thermal property of composite material, filler
Hybridism it is increasing.In Chinese invention patent 201310629967.1, with graphene and Al2O3For heat filling, prepare
Graphene/Al2O3/ silicon rubber composite material, compared with silicon rubber is the thermal coefficient of 0.16W/ (mK), the composite material
Thermal coefficient reaches 1.49W/ (mK).In this approach, graphene and Al2O3It is unprocessed, dosage in silicon rubber compared with
It is more, and they are very poor with the compatibility of silicon rubber.In 104327515 A of Chinese invention patent CN, with modified graphene and table
Modified material of the inorganic particulate as silicon rubber that face is modified, the thermal coefficient of the silicon rubber of preparation at 40 DEG C is 4.98W/
(mK), in the method, as two independent heat conduction networks, the collaboration for being not carried out the two is made for graphene and inorganic particulate
With the sharpest edges of two kinds of materials cannot be given full play to.Generally for making the thermal coefficient of silicon rubber reach 1.5W/ (mK),
The adding proportion of heat filling is up to 50~70wt%.Although a high proportion of heat filling can improve the heat conduction system of silicon rubber
Number, but its mechanical property is caused to be deteriorated.
Invention content
The purpose of the present invention is to provide a kind of preparation sides of the high thermal conductive silicon rubber of nitrogen aluminium/graphene hybrid material
Method.3-aminopropyltriethoxysilane is modified aluminium nitride first by the present invention and glycidyl 3- trimethoxy silicon substrate propyl ether changes
Property graphene chemically reacted, prepare nitride aluminum/graphite alkene hybrid material, then add the hybrid material as heat filling
Into silicon rubber, the silicon rubber with excellent toughness and elasticity, excellent heat conductivity is prepared.
To achieve the above object, preparation method of the invention includes the following steps：
(1) under the action of ultrasound, modified aluminium nitride and modified graphene are reacted, and it is miscellaneous to prepare nitride aluminum/graphite alkene
Change material；
(2) hybrid material, softening agent and anti-aging agent prepared by step (1) are added sequentially in silicon rubber, utilize mill
Machine is kneaded, and rubber compound is prepared；
(3) rubber compound for preparing step (2) it is thin it is logical for several times, it is thin it is logical during crosslinking agent is added, passed through after thin pass-out piece
Vulcanization prepares vulcanizate, the high thermal conductive silicon rubber of as described nitrogen aluminium/graphene hybrid material.
More specifically steps are as follows：
(1) 1~10g 3-aminopropyltriethoxysilane is modified aluminium nitride (Yan Dong conductions/heat conducting nano composite wood
The preparation of material and performance study [D] Beijing University of Chemical Technology, 2013) and 2~200mg glycidyl 3- trimethoxy silicon substrate propyl ether
(Chen Jianjian, Yu Kejing, Qian Kun, Cao Hai build synthetic fiber industries, 2012,35 (6) to modified graphene：12-16) it is added to 50~
In 300mL toluene, after 15~30min of room temperature ultrasound, 70~90 DEG C are warming up to, reacts 4~12h, product is washed through filtering, ethyl alcohol
It washs, is dried in vacuo at 60 DEG C for 24 hours, prepare nitride aluminum/graphite alkene hybrid material；
(2) hybrid material, 6~10 parts of softening agents, 3~6 parts of anti-aging agents prepared by 25~55 parts of steps (1) are sequentially added
Into 100 parts of silicon rubber, utilizes two-roll mill to be kneaded 30~60min at room temperature, be placed at room temperature for for 24 hours, prepare rubber compound；
(3) rubber compound for preparing step (2) utilizes two-roll mill thin 4~8 times logical at room temperature, during thin logical
1~3 part of crosslinking agent is added, is vulcanized using vulcanizing press, prepares vulcanizate, as described nitrogen aluminium/graphene is miscellaneous
Change the high thermal conductive silicon rubber of material.
The power of the ultrasonic wave is 200W.
The softening agent is any one in aromatic naphtha, paraffin or vaseline.
The anti-aging agent is in N- phenyl-α-naphthylamines, N- phenyl-N '-cyclohexyl p-phenylenediamine or calcium-zinc composite stabilizing agent
Any one.
The crosslinking agent is arbitrary in cumyl peroxide, benzoyl peroxide, 2,4- dichlorobenzoperoxides
It is a kind of.
100~170 DEG C of curing temperature；10~15MPa of sulfide stress；10~20min of vulcanization time.
The present invention preparation method and obtained product has the following advantages that and advantageous effect：
1. the invention has used nitride aluminum/graphite alkene hybrid material as the heat filling of silicon rubber, change
The preparation method of previous single filler or two kinds of independent fillers.
2. one side because of the effect of graphene, aluminium nitride are not susceptible to reunite, is on the other hand distributed on the surface of graphene
On aluminium nitride play the role of isolation, can also effectively prevent the reunion of graphene sheet layer, the collaboration dispersion effect of the two is aobvious
It writes.
3. the organic matter on hybrid material can improve the compatibility of hybrid material and silicon rubber, is conducive to hybrid material and exists
It is evenly dispersed in silicon rubber, form good heat conduction network.
4. the heat filling of lower content can increase substantially the thermal conductivity of silicon rubber, the heat filling of high-content is avoided
Destruction to silicon rubber elastic.Meanwhile the laminar structured of graphene can also impart to the good toughness of silicon rubber.
Specific implementation mode
With reference to example, the present invention is described in further detail, and embodiments of the present invention are not limited thereto.
Embodiment 1
(1) 1g 3-aminopropyltriethoxysilane is modified aluminium nitride and 2mg glycidyl 3- trimethoxies silicon substrate third
Ether modified graphene is added in 50mL toluene, after room temperature ultrasound 15min, is warming up to 70 DEG C, reacts 12h, product is through filtering, second
Alcohol washs, and is dried in vacuo at 60 DEG C for 24 hours, prepares nitride aluminum/graphite alkene hybrid material；
(2) hybrid material, 6 parts of aromatic naphtha, 3 parts of N- phenyl-α-naphthylamines prepared by 25 parts of steps (1) are added to 100 parts
In silicon rubber, utilizes two-roll mill to be kneaded 30min at room temperature, be placed at room temperature for for 24 hours, prepare rubber compound；
(3) it utilizes two-roll mill thin 4 times logical at room temperature the rubber compound of step (2) preparation, adds during thin lead to
Enter 3 parts of cumyl peroxides, is vulcanized using vulcanizing press, 100 DEG C, sulfide stress 15MPa of curing temperature, when vulcanization
Between 20min, prepare vulcanizate, the high thermal conductive silicon rubber of as described nitrogen aluminium/graphene hybrid material.
Embodiment 2
(1) 5g 3-aminopropyltriethoxysilane is modified aluminium nitride and 25mg glycidyl 3- trimethoxy silicon substrates
Propyl ether modified graphene is added in 90mL toluene, after room temperature ultrasound 20min, is warming up to 80 DEG C, reacts 8h, product through filtering,
Ethyl alcohol washs, and is dried in vacuo 12h at 60 DEG C, prepares nitride aluminum/graphite alkene hybrid material；
(2) hybrid material, 7 parts of paraffin, 4 parts of N- phenyl-N '-cyclohexyl p-phenylenediamine prepared by 40 parts of steps (1) are added
Enter into 100 parts of silicon rubber, utilizes two-roll mill to be kneaded 30min at room temperature, be placed at room temperature for for 24 hours, prepare rubber compound；
(3) it utilizes two-roll mill thin 6 times logical at room temperature the rubber compound of step (2) preparation, adds during thin lead to
Enter 2 parts of benzoyl peroxides, is vulcanized using vulcanizing press, 140 DEG C, sulfide stress 12MPa of curing temperature, vulcanization time
15min prepares vulcanizate, the high thermal conductive silicon rubber of as described nitrogen aluminium/graphene hybrid material.
Example example 3
(1) 10g 3-aminopropyltriethoxysilane is modified aluminium nitride and 200mg glycidyl 3- trimethoxy silicon
Base propyl ether modified graphene is added in 300mL toluene, after room temperature ultrasound 30min, is warming up to 90 DEG C, reacts 4h, and product passes through
Filter, ethyl alcohol washing, are dried in vacuo for 24 hours at 60 DEG C, prepare nitride aluminum/graphite alkene hybrid material；
(2) hybrid material, 9 parts of vaseline, 6 parts of calcium-zinc composite stabilizing agents prepared by 55 parts of steps (1) are added sequentially to
In 100 parts of silicon rubber, utilizes two-roll mill to be kneaded 60min at room temperature, be placed at room temperature for for 24 hours, prepare rubber compound；
(3) it utilizes two-roll mill thin 8 times logical at room temperature the rubber compound of step (2) preparation, adds during thin lead to
Enter 1 part of 2,4- dichlorobenzoperoxide, is vulcanized using vulcanizing press, 170 DEG C, sulfide stress 10MPa of curing temperature,
Vulcanization time 10min prepares vulcanizate, the high thermal conductive silicon rubber of as described nitrogen aluminium/graphene hybrid material.
Comparative example 1
(1) 1g aluminium nitride and 2mg graphenes is taken to be added in the toluene of 50ml under room temperature, room temperature ultrasound 15min is warming up to
70 DEG C, 12h is reacted, product is washed through filtering, ethyl alcohol, is dried in vacuo at 60 DEG C for 24 hours, and it is mixed that nitride aluminum/graphite alkene is prepared
Close filler；
(2) hybrid material, 6 parts of aromatic naphtha, 3 parts of N- phenyl-α-naphthylamines prepared by 25 parts of steps (1) are added to 100 parts
In silicon rubber, utilizes two-roll mill to be kneaded 30min at room temperature, be placed at room temperature for for 24 hours, prepare rubber compound；
(3) it utilizes two-roll mill thin 4 times logical at room temperature the rubber compound of step (2) preparation, adds during thin lead to
Enter 3 parts of cumyl peroxides, is vulcanized using vulcanizing press, 100 DEG C, sulfide stress 15MPa of curing temperature, when vulcanization
Between 20min, prepare vulcanizate, the high thermal conductive silicon rubber of as described nitrogen aluminium/graphene hybrid material.
Comparative example 2
(1) 5g aluminium nitride and 25mg graphenes is taken to be added in the toluene of 90ml under room temperature, room temperature ultrasound 20min, heating
To 80 DEG C, 8h is reacted, product is washed through filtering, ethyl alcohol, is dried in vacuo 12h at 60 DEG C, it is mixed that nitride aluminum/graphite alkene is prepared
Close filler；
(2) hybrid material, 7 parts of paraffin, 4 parts of N- phenyl-N '-cyclohexyl p-phenylenediamine prepared by 40 parts of steps (1) are added
Enter into 100 parts of silicon rubber, utilizes two-roll mill to be kneaded 30min at room temperature, be placed at room temperature for for 24 hours, prepare rubber compound；
(3) it utilizes two-roll mill thin 6 times logical at room temperature the rubber compound of step (2) preparation, adds during thin lead to
Enter 2 parts of benzoyl peroxides, is vulcanized using vulcanizing press, 140 DEG C, sulfide stress 12MPa of curing temperature, vulcanization time
15min prepares vulcanizate, the high thermal conductive silicon rubber of as described nitrogen aluminium/graphene hybrid material.
Comparative example 3
(1) 10g aluminium nitride and 200mg graphenes is taken to be added in the toluene of 300ml under room temperature, after room temperature ultrasound 30min,
90 DEG C are warming up to, 4h is reacted, product washs through filtering, ethyl alcohol, is dried in vacuo at 60 DEG C for 24 hours, nitride aluminum/graphite is prepared
Alkene mixed fillers；
(2) hybrid material, 9 parts of vaseline, 6 parts of calcium-zinc composite stabilizing agents prepared by 55 parts of steps (1) are added sequentially to
In 100 parts of silicon rubber, utilizes two-roll mill to be kneaded 60min at room temperature, be placed at room temperature for for 24 hours, prepare rubber compound；
(3) it utilizes two-roll mill thin 8 times logical at room temperature the rubber compound of step (2) preparation, adds during thin lead to
Enter 1 part of 2,4- dichlorobenzoperoxide, is vulcanized using vulcanizing press, 170 DEG C, sulfide stress 10MPa of curing temperature,
Vulcanization time 10min prepares vulcanizate, the high thermal conductive silicon rubber of as described nitrogen aluminium/graphene hybrid material.
Silicon rubber obtained in three groups of embodiments and three groups of comparative examples is subjected to impact strength according to GB/T 1843-1996
Test, elongation at break test is carried out according to GB/T 1701-2001, and elasticity modulus test is carried out according to GB/T 528-2009,
Heat conductivility test is carried out according to ASTM D5470, test result is as follows shown in table.
It can be seen that from the test result of three groups of embodiments and three groups of comparative examples and be directly added into aluminium nitride and graphene phase
Than, nitride aluminum/graphite alkene hybrid material is added in silicon rubber, can more efficiently improve silicon rubber thermal coefficient and
Impact strength reduces the reduction amplitude of elongation at break and elasticity modulus.
The preferred embodiment of the present invention has shown and described in above description, as previously described, it should be understood that the present invention is not office
Be limited to form disclosed herein, be not to be taken as excluding other embodiments, and can be used for various other combinations, modification and
Environment, and can be changed by the above teachings or related fields of technology or knowledge in the scope of the invention is set forth herein
It is dynamic.And changes and modifications made by those skilled in the art do not depart from the spirit and scope of the present invention, then it all should be appended by the present invention
In scope of the claims.
Claims (7)
1. a kind of preparation method of the high thermal conductive silicon rubber of nitrogen aluminium/graphene hybrid material, it is characterised in that：Including following
Step：
(1) under the action of ultrasound, modified aluminium nitride and modified graphene are reacted, and nitride aluminum/graphite alkene hydridization material is prepared
Material；
(2) by step (1) prepare hybrid material, softening agent and anti-aging agent be added sequentially in silicon rubber, using open mill into
Row is kneaded, and prepares rubber compound；
(3) rubber compound for preparing step (2) it is thin it is logical for several times, it is thin it is logical during be added crosslinking agent, through vulcanization after thin pass-out piece
Prepare vulcanizate, the high thermal conductive silicon rubber of as described nitrogen aluminium/graphene hybrid material.
2. the preparation method of the high thermal conductive silicon rubber of nitrogen aluminium/graphene hybrid material according to claim 1, special
Sign is：It is as follows：
(1) 1~10g 3-aminopropyltriethoxysilane is modified aluminium nitride and 2~200mg glycidyl 3- trimethoxies
Silicon substrate propyl ether modified graphene is added in 50~300mL toluene, after 15~30min of room temperature ultrasound, is warming up to 70~90 DEG C, is surpassed
4~12h of phonoresponse, product wash through filtering, ethyl alcohol, are dried in vacuo at 60 DEG C for 24 hours, prepare nitride aluminum/graphite alkene hydridization material
Material；
(2) hybrid material, 6~10 parts of softening agents, 3~6 parts of anti-aging agents prepared by 25~55 parts of steps (1) are added sequentially to
In 100 parts of silicon rubber, utilizes two-roll mill to be kneaded 30~60min at room temperature, be placed at room temperature for for 24 hours, prepare rubber compound；
(3) rubber compound for preparing step (2) utilizes two-roll mill thin 4~8 times logical at room temperature, is added during thin lead to
1~3 part of crosslinking agent, is vulcanized using vulcanizing press, prepares vulcanizate, as described nitrogen aluminium/graphene hydridization material
The high thermal conductive silicon rubber of material.
3. the preparation method of the high thermal conductive silicon rubber of nitrogen aluminium/graphene hybrid material according to claim 1 and 2,
It is characterized in that：The power of the ultrasonic wave is 200W.
4. the preparation method of the high thermal conductive silicon rubber of nitrogen aluminium/graphene hybrid material according to claim 1 and 2,
It is characterized in that：The softening agent is any one in aromatic naphtha, paraffin or vaseline.
5. the preparation method of the high thermal conductive silicon rubber of nitrogen aluminium/graphene hybrid material according to claim 1 and 2,
It is characterized in that：The anti-aging agent is N- phenyl-α-naphthylamines, N- phenyl-N '-cyclohexyl p-phenylenediamine or calcium-zinc composite stabilizing agent
In any one.
6. the preparation method of the high thermal conductive silicon rubber of nitrogen aluminium/graphene hybrid material according to claim 1 and 2,
It is characterized in that：The crosslinking agent is appointing in cumyl peroxide, benzoyl peroxide, 2,4- dichlorobenzoperoxides
Meaning is a kind of.
7. the preparation method of the high thermal conductive silicon rubber of nitrogen aluminium/graphene hybrid material according to claim 1 and 2,
It is characterized in that：100~170 DEG C of curing temperature；10~15MPa of sulfide stress；10~20min of vulcanization time.
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| CN114591636A (en) * | 2022-01-22 | 2022-06-07 | 中北大学 | Vulcanizing agent modified graphene prepared by chemical in-situ deposition process and controllable cross-linked natural rubber composite material thereof |
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