CN108822532A - Graphene nylon composite materials and preparation method thereof - Google Patents
Graphene nylon composite materials and preparation method thereof Download PDFInfo
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- CN108822532A CN108822532A CN201810753557.0A CN201810753557A CN108822532A CN 108822532 A CN108822532 A CN 108822532A CN 201810753557 A CN201810753557 A CN 201810753557A CN 108822532 A CN108822532 A CN 108822532A
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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
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
Abstract
The invention proposes a kind of graphene nylon composite materials and preparation method thereof, according to the number of parts by weight, including following raw material：70~90 parts of nylon, 5~10 parts of carbon fiber, 20~30 parts of modified graphene, 4~8 parts of toughener, 0.6~1.8 part of compatilizer, 0.2~0.6 part of lubricant and 0.2~0.6 part of antioxidant；The modified graphene is mainly prepared by graphene, citric acid and sodium metaaluminate.Preparation method：Double-screw extruding pelletizing is carried out after above-mentioned raw materials are mixed in batches.The nylon composite materials not only have extraordinary heat-conducting effect, other mechanical properties are also very excellent.
Description
Technical field
The invention belongs to technical field of polymer materials, and in particular to a kind of graphene nylon composite materials and its preparation side
Method.
Background technique
Nylon has excellent comprehensive such as good mechanical performance, preferable flexibility, wearability, oil resistivity, self-lubrication
Performance is closed, the fields such as automobile industry, electronic apparatus industry, mechanical equipment, construction industry are widely used in.Since it has processing
The advantages that period is short, production cost is low, long service life and product design freedom degree are high has been more and more widely used, close several
Year in terms of heat-conductivity polymer composite using especially prominent, such as the high-power LED radiator of Royal DSM company production
The generally approval in market is obtained.
Heat Conduction Material is widely used in the fields such as engineering, Electronics and Information Engineering that exchange heat.For a long time, most of Heat Conduction Material
For metal material, but since the corrosion resistance of metal material difference and processing performance are bad, product design freedom degree is low etc.
Factors limit its scope of application.
In order to improve the surface erosion resistance of Heat Conduction Material, the means such as metallurgy, corrosion-inhibiting coating are generallyd use, but the method
Other performances for largely reducing the heating conduction of material and material do not obtain the improvement of essence.In recent years
Come, as Heat Conduction Material will be used wider and wider general, the comprehensive performance of material is required also higher and higher.For example it does not require nothing more than
Material has excellent heating conduction, and material is also required to have good mechanical performance, high temperature resistant service performance, environmental corrosion resisting
Performance etc..
Traditional heat-conductive composite material is generally with Si3N4, SiN, AlN and BN as heat filling, but leading because of itself
Heating rate is low, therefore higher thermal coefficient need to could be obtained under high additive amount, however this will necessarily reduce high molecular material sheet
Other performances of body.
Summary of the invention
The present invention proposes that a kind of graphene nylon composite materials, the nylon composite materials not only have extraordinary thermally conductive effect
Fruit, other mechanical properties are also very excellent.
The technical proposal of the invention is realized in this way：
A kind of graphene nylon composite materials, according to the number of parts by weight, including following raw material：
70~90 parts of nylon, 5~10 parts of carbon fiber, 20~30 parts of modified graphene, 4~8 parts of toughener, compatilizer 0.6
~1.8 parts, 0.2~0.6 part of lubricant and 0.2~0.6 part of antioxidant；The modified graphene is mainly by graphene, lemon
Acid is prepared with sodium metaaluminate.
Preferably, the preparation method of the modified graphene include can following steps：
1) graphene is added in the alcoholic solution of citric acid and carries out ultrasonic disperse, obtain the alcohol dispersion of carboxylated graphene
Liquid；
2) sodium metaaluminate is added into the alcohol dispersion liquid of carboxylated graphene, then is stirred to react, after reaction from
Heart filtering, obtains filtrate；
3) by filtrate under the conditions of nitrogen atmosphere, 400~600 DEG C are warming up to the heating rate of 1~5 DEG C/min, and
Keep the temperature 1~3h.
Preferably, the mass ratio of the graphene and the citric acid is 1:2~6, the graphene and the inclined aluminium
The mass ratio of sour sodium is 1:3~7.
Preferably, the alcoholic solution is ethanol solution, propanol solution or butanol solution.
Preferably, the toughener is selected from maleic anhydride grafted ethene-octene copolymer, glycidyl methacrylate
At least one of grafted ethene-octene copolymer.
Preferably, the compatilizer in for styrene-maleic anhydride copolymer, maleic anhydride grafted polyphenylene ether extremely
Few one kind.
Preferably, the antioxidant is at least one of Hinered phenols, thioesters, phosphite ester antioxidant.
Preferably, the lubricant is polyethylene wax, stearate, ethylene bis stearamide, grafting ethylene stearic bicine diester
At least one of amine.
Another object of the present invention provides a kind of preparation method of graphene nylon composite materials, includes the following steps：
1) weigh according to the proportion 70~90 parts of nylon, 5~10 parts of carbon fiber, 20~30 parts of modified graphene, toughener 4~
8 parts, 0.6~1.8 part of compatilizer, 0.2~0.6 part of lubricant and 0.2~0.6 part of antioxidant are spare；
2) nylon, toughener, carbon fiber and modified graphene are mixed evenly, are then added to double screw extruder
In, extruding pelletization is carried out under the conditions of 250~270 DEG C, obtains thermally conductive nylon master batch；
3) the thermally conductive nylon master batch of step 2) is dried, then again with organosilicon modified polyester acrylate, compatible
Agent, antioxidant and mix lubricant stir evenly, and obtain mixed material；
4) mixed material of step 3) is added in double screw extruder, carries out squeezing out under the conditions of 260~280 DEG C and makes
Grain.
Beneficial effects of the present invention：
The present invention, can be with by selecting the modified graphene that is mainly prepared by graphene, citric acid and sodium metaaluminate
It is evenly dispersed into matrix resin very much, so that the interface cohesive force between modified graphene and nylon becomes strong, compatibility is high, and
And it is coated on the surface of nylon particle well, form preferable passage of heat.
Specific embodiment
Embodiment 1
The preparation method of modified graphene includes can following steps：
1) graphene is added in the ethanol solution of citric acid and carries out ultrasonic disperse, obtain the alcohol point of carboxylated graphene
Dispersion liquid；
2) sodium metaaluminate is added into the alcohol dispersion liquid of carboxylated graphene, then is stirred to react, after reaction from
Heart filtering, obtains filtrate；
3) by filtrate under the conditions of nitrogen atmosphere, 400 DEG C are warming up to the heating rate of 1 DEG C/min, and keep the temperature 3h, i.e.,
It can.The mass ratio of graphene and citric acid is 1:6, the mass ratio of graphene and sodium metaaluminate is 1:3.
Embodiment 2
The preparation method of modified graphene includes can following steps：
1) graphene is added in the propanol solution of citric acid and carries out ultrasonic disperse, obtain the alcohol point of carboxylated graphene
Dispersion liquid；
2) sodium metaaluminate is added into the alcohol dispersion liquid of carboxylated graphene, then is stirred to react, after reaction from
Heart filtering, obtains filtrate；
3) by filtrate under the conditions of nitrogen atmosphere, 600 DEG C are warming up to the heating rate of 5 DEG C/min, and keep the temperature 1h, i.e.,
It can.The mass ratio of graphene and citric acid is 1:2, the mass ratio of graphene and sodium metaaluminate is 1:7.
Embodiment 3
A kind of graphene nylon composite materials, according to the number of parts by weight, including following raw material：
0 part of nylon 8,7 parts of carbon fiber, embodiment 1 24 parts of modified graphene, maleic anhydride grafted ethene-octene copolymer
6 parts of object, 1.2 parts of styrene-maleic anhydride copolymer, 0.4 part of polyethylene wax and 0.4 part of hindered phenol anti-oxidants.
The preparation method of graphene nylon composite materials：
1) nylon, maleic anhydride grafted ethene-octene copolymer, carbon fiber are mixed with the modified graphene of embodiment 1
It stirs evenly, is then added in double screw extruder, carry out extruding pelletization under the conditions of 260 DEG C, obtain thermally conductive nylon master batch；
2) the thermally conductive nylon master batch of step 1) is dried, then again with styrene-maleic anhydride copolymer, hindered phenol
Class antioxidant is mixed evenly with polyethylene wax, obtains mixed material；
3) mixed material of step 2) is added in double screw extruder, carries out extruding pelletization under the conditions of 270 DEG C, i.e.,
It can.
Embodiment 4
A kind of graphene nylon composite materials, according to the number of parts by weight, including following raw material：
70 parts of nylon, 5 parts of carbon fiber, 20 parts of the modified graphene of embodiment 2, glycidyl methacrylate graft second
8 parts of alkene-octene copolymer, 0.6 part of maleic anhydride grafted polyphenylene ether, 0.2 part of ethylene bis stearamide and thioesters are anti-oxidant
0.2 part of agent.
The preparation method of graphene nylon composite materials：
1) changing nylon, glycidyl methacrylate graft ethylene-octene copolymer, carbon fiber and embodiment 2
Property graphene is mixed evenly, and is then added in double screw extruder, extruding pelletization is carried out under the conditions of 250 DEG C, obtain
Thermally conductive nylon master batch；
2) the thermally conductive nylon master batch of step 1) is dried, then again with maleic anhydride grafted polyphenylene ether, thioesters
Antioxidant is mixed evenly with ethylene bis stearamide, obtains mixed material；
3) mixed material of step 2) is added in double screw extruder, carries out extruding pelletization under the conditions of 260 DEG C, i.e.,
It can.
Embodiment 5
A kind of graphene nylon composite materials, according to the number of parts by weight, including following raw material：
0 part of nylon 9,10 parts of carbon fiber, embodiment 1 30 parts of modified graphene, maleic anhydride grafted ethene-octene copolymer
4 parts of object, 1.8 parts of styrene-maleic anhydride copolymer, 0.6 part of zinc stearate and 0.6 part of phosphite antioxidant.
The preparation method of graphene nylon composite materials：
1) nylon, maleic anhydride grafted ethene-octene copolymer, carbon fiber are mixed with the modified graphene of embodiment 1
It stirs evenly, is then added in double screw extruder, carry out extruding pelletization under the conditions of 270 DEG C, obtain thermally conductive nylon master batch；
2) the thermally conductive nylon master batch of step 1) is dried, then again with styrene-maleic anhydride copolymer, phosphorous acid
Esters antioxidant is mixed evenly with zinc stearate, obtains mixed material；
3) mixed material of step 2) is added in double screw extruder, carries out extruding pelletization under the conditions of 280 DEG C, i.e.,
It can.
Test example
The graphene nylon composite materials of embodiment 3-5 are tested for the property, the results are shown in Table 1.
The graphene nylon composite materials the performance test results of 1 embodiment 3-5 of table
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (9)
1. a kind of graphene nylon composite materials, which is characterized in that according to the number of parts by weight, including following raw material：
70~90 parts of nylon, 5~10 parts of carbon fiber, 20~30 parts of modified graphene, 4~8 parts of toughener, compatilizer 0.6~1.8
Part, 0.2~0.6 part of lubricant and 0.2~0.6 part of antioxidant；The modified graphene mainly by graphene, citric acid and partially
Sodium aluminate is prepared.
2. graphene nylon composite materials according to claim 1, which is characterized in that the preparation side of the modified graphene
Method includes can following steps：
1) graphene is added in the alcoholic solution of citric acid and carries out ultrasonic disperse, obtain the alcohol dispersion liquid of carboxylated graphene；
2) sodium metaaluminate is added into the alcohol dispersion liquid of carboxylated graphene, then is stirred to react, be centrifuged after reaction
Filter, obtains filtrate；
3) by filtrate under the conditions of nitrogen atmosphere, 400~600 DEG C are warming up to the heating rate of 1~5 DEG C/min, and keep the temperature 1
~3h.
3. graphene nylon composite materials according to claim 2, which is characterized in that the graphene and the citric acid
Mass ratio be 1:2~6, the mass ratio of the graphene and the sodium metaaluminate is 1:3~7.
4. graphene nylon composite materials according to claim 2, which is characterized in that the alcoholic solution be ethanol solution,
Propanol solution or butanol solution.
5. graphene nylon composite materials according to claim 1, which is characterized in that the toughener is selected from maleic anhydride
At least one of grafted ethene-octene copolymer, glycidyl methacrylate graft ethylene-octene copolymer.
6. graphene nylon composite materials according to claim 1, which is characterized in that it is benzene second that the compatilizer, which is selected from,
At least one of alkene-copolymer-maleic anhydride, maleic anhydride grafted polyphenylene ether.
7. graphene nylon composite materials according to claim 1, which is characterized in that the antioxidant be Hinered phenols,
At least one of thioesters, phosphite ester antioxidant.
8. graphene nylon composite materials according to claim 1, which is characterized in that the lubricant be polyethylene wax,
At least one of stearate, ethylene bis stearamide, grafting ethylene bis stearamide.
9. the preparation method of graphene nylon composite materials as described in claim 1, which is characterized in that include the following steps：
1) weigh according to the proportion 70~90 parts of nylon, 5~10 parts of carbon fiber, 20~30 parts of modified graphene, 4~8 parts of toughener,
0.6~1.8 part of compatilizer, 0.2~0.6 part of lubricant and 0.2~0.6 part of antioxidant are spare；
2) nylon, toughener, carbon fiber and modified graphene are mixed evenly, are then added in double screw extruder,
Extruding pelletization is carried out under the conditions of 250~270 DEG C, obtains thermally conductive nylon master batch；
3) the thermally conductive nylon master batch of step 2) is dried, then again with organosilicon modified polyester acrylate, compatilizer, anti-
Oxidant is stirred evenly with mix lubricant, obtains mixed material；
4) mixed material of step 3) is added in double screw extruder, carries out extruding pelletization under the conditions of 260~280 DEG C,
?.
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| CN201810753557.0A CN108822532A (en) | 2018-07-10 | 2018-07-10 | Graphene nylon composite materials and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109735097A (en) * | 2018-11-23 | 2019-05-10 | 陕西省石油化工研究设计院 | A kind of low water suction High impact nylon composite material and preparation method |
| CN110079083A (en) * | 2019-05-28 | 2019-08-02 | 烟台恒大聚合体有限公司 | Nylon 66 composite material and preparation method thereof for link rod sleeve |
| CN113995189A (en) * | 2021-11-24 | 2022-02-01 | 安徽高梵电子商务有限公司 | Preparation method of graphene antibacterial down jacket fabric |
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| CN103951974A (en) * | 2014-05-15 | 2014-07-30 | 平顶山华邦工程塑料有限公司 | Anti-static heat-conducting nylon composite material and preparation method for same |
| CN103951973A (en) * | 2014-05-12 | 2014-07-30 | 安徽孟凌精密电子有限公司 | Graphite fibre nylon formula |
| CN106633827A (en) * | 2016-12-29 | 2017-05-10 | 宁波墨西科技有限公司 | Graphene nylon composite material and preparation method thereof |
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2018
- 2018-07-10 CN CN201810753557.0A patent/CN108822532A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103951973A (en) * | 2014-05-12 | 2014-07-30 | 安徽孟凌精密电子有限公司 | Graphite fibre nylon formula |
| CN103951974A (en) * | 2014-05-15 | 2014-07-30 | 平顶山华邦工程塑料有限公司 | Anti-static heat-conducting nylon composite material and preparation method for same |
| CN106633827A (en) * | 2016-12-29 | 2017-05-10 | 宁波墨西科技有限公司 | Graphene nylon composite material and preparation method thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109735097A (en) * | 2018-11-23 | 2019-05-10 | 陕西省石油化工研究设计院 | A kind of low water suction High impact nylon composite material and preparation method |
| CN110079083A (en) * | 2019-05-28 | 2019-08-02 | 烟台恒大聚合体有限公司 | Nylon 66 composite material and preparation method thereof for link rod sleeve |
| CN113995189A (en) * | 2021-11-24 | 2022-02-01 | 安徽高梵电子商务有限公司 | Preparation method of graphene antibacterial down jacket fabric |
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