CN109082113A - Fiber reinforced nylon composite material and preparation method thereof - Google Patents
Fiber reinforced nylon composite material and preparation method thereof Download PDFInfo
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- CN109082113A CN109082113A CN201810752085.7A CN201810752085A CN109082113A CN 109082113 A CN109082113 A CN 109082113A CN 201810752085 A CN201810752085 A CN 201810752085A CN 109082113 A CN109082113 A CN 109082113A
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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
- C08L77/06—Polyamides derived from polyamines and polycarboxylic acids
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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
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
- C08L2205/16—Fibres; Fibrils
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Abstract
The invention proposes a kind of fiber reinforced nylon composite materials and preparation method thereof, according to the number of parts by weight, including following raw material: 60~80 parts of nylon, 10~20 parts of organosilicon modified polyester acrylate, 5~10 parts of aramid 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, oxalic 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, additionally it is possible to be resistant to very high temperature, 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 fiber reinforced nylon composite material and its preparation
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.
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..
The thermal coefficient of nylon66 fiber is generally 0.25W (mK) -1, greatly limits it and answers in heat dissipation, thermally conductive field
With.Therefore, how overcome the deficiencies in the prior art, producing enhanced thermal conduction type nylon 66 composite material is current the field of polymers
The problem of urgent need to resolve.Traditional heat-conductive composite material is generally with Si3N4, SiN, AlN and BN as heat filling, but Yin Qiben
The thermal conductivity of body is low, therefore higher thermal coefficient need to could be obtained under high additive amount, however this will necessarily reduce macromolecule
Other performances of material itself.
Summary of the invention
The present invention proposes a kind of fiber reinforced nylon composite material, which not only has extraordinary thermally conductive
Effect, additionally it is possible to be resistant to very high temperature, other mechanical properties are also very excellent.
The technical scheme of the present invention is realized as follows:
A kind of fiber reinforced nylon composite material, according to the number of parts by weight, including following raw material:
60~80 parts of nylon66 fiber, 10~20 parts of organosilicon modified polyester acrylate, 5~10 parts of aramid fiber, modified stone
20~30 parts of black alkene, 4~8 parts of toughener, 0.6~1.8 part of compatilizer, 0.2~0.6 part of lubricant and antioxidant 0.2~0.6
Part；The modified graphene is mainly prepared by graphene, oxalic acid and sodium metaaluminate.
Preferably, the preparation method of the modified graphene include can following steps:
1) graphene is added in the alcoholic solution of oxalic 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 oxalic acid is 1:2~6, the graphene and the meta-aluminic acid
The mass ratio of 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 fiber reinforced nylon composite material, including following step
It is rapid:
1) 60~80 parts of nylon66 fiber, 10~20 parts of organosilicon modified polyester acrylate, aramid fiber are weighed according to the proportion
5~10 parts, 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 anti-
0.2~0.6 part of oxidant spare；
2) nylon66 fiber, toughener, aramid fiber and modified graphene are mixed evenly, are then added to twin-screw and squeeze
Out in machine, 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:
1, the present invention selects organosilicon modified polyester acrylate as reinforced resin, is a kind of polymer three-dimensional Cross-linked
Object is closed, film is in rigidity, and thermal coefficient is smaller, and heat-resisting quantity is good, and water impermeability is excellent, and adhesive force is strong, but Low temperature-resistanflexible flexible
Difference.Itself and nylon cooperate, and improve the structure of nylon, form more tridimensional networks between them, facilitate aramid fiber
Disperse wherein with modified graphene, substantially increases its thermal coefficient and mechanical property.
2, the present invention is by the modified graphene that is mainly prepared by graphene, oxalic acid and sodium metaaluminate of selection, can be with
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 oxalic 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 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 oxalic acid is 1:6, and 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 oxalic 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, 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 oxalic acid is 1:2, and the mass ratio of graphene and sodium metaaluminate is 1:7.
Embodiment 3
A kind of fiber reinforced nylon composite material, according to the number of parts by weight, including following raw material:
70 parts of nylon66 fiber, 14 parts of organosilicon modified polyester acrylate, 7 parts of aramid fiber, embodiment 1 modified graphite
24 parts of alkene, 6 parts of maleic anhydride grafted ethene-octene copolymer, 1.2 parts of styrene-maleic anhydride copolymer, polyethylene wax 0.4
Part and 0.4 part of hindered phenol anti-oxidants.
The preparation method of fiber reinforced nylon composite material:
1) by nylon66 fiber, maleic anhydride grafted ethene-octene copolymer, aramid fiber and embodiment 1 modified graphene
It is mixed 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 organosilicon modified polyester acrylate, benzene second
Alkene-copolymer-maleic anhydride, hindered phenol anti-oxidants and polyethylene wax are mixed evenly, and obtain 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 fiber reinforced nylon composite material, according to the number of parts by weight, including following raw material:
60 parts of nylon66 fiber, 20 parts of organosilicon modified polyester acrylate, 5 parts of aramid fiber, embodiment 2 modified graphite
20 parts of alkene, 8 parts of glycidyl methacrylate graft ethylene-octene copolymer, 0.6 part of maleic anhydride grafted polyphenylene ether, second
Support 0.2 part of bis-stearamides and 0.2 part of thioesters antioxidant.
The preparation method of fiber reinforced nylon composite material:
1) by nylon66 fiber, glycidyl methacrylate graft ethylene-octene copolymer, aramid fiber and embodiment 2
Modified graphene be mixed evenly, be then added in double screw extruder, carry out extruding pelletization 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 organosilicon modified polyester acrylate, Malaysia
Acid anhydrides grafted polyphenylene ether, thioesters antioxidant and ethylene bis stearamide are mixed evenly, and obtain 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 fiber reinforced nylon composite material, according to the number of parts by weight, including following raw material:
80 parts of nylon66 fiber, 10 parts of organosilicon modified polyester acrylate, 10 parts of aramid fiber, embodiment 1 modified graphite
30 parts of alkene, 4 parts of maleic anhydride grafted ethene-octene copolymer, 1.8 parts of styrene-maleic anhydride copolymer, zinc stearate 0.6
Part and 0.6 part of phosphite antioxidant.
The preparation method of fiber reinforced nylon composite material:
1) by nylon66 fiber, maleic anhydride grafted ethene-octene copolymer, aramid fiber and embodiment 1 modified graphene
It is mixed 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 organosilicon modified polyester acrylate, benzene second
Alkene-copolymer-maleic anhydride, phosphite antioxidant and zinc stearate are mixed evenly, and obtain 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 fiber reinforced nylon composite material of embodiment 3-5 is tested for the property, the results are shown in Table 1.
The fiber reinforced nylon composite material 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 fiber reinforced nylon composite material, which is characterized in that according to the number of parts by weight, including following raw material:
60~80 parts of nylon66 fiber, 10~20 parts of organosilicon modified polyester acrylate, 5~10 parts of aramid fiber, modified graphene
20~30 parts, 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, oxalic acid and sodium metaaluminate.
2. fiber reinforced nylon composite material according to claim 1, which is characterized in that the preparation of the modified graphene
Method includes can following steps:
1) graphene is added in the alcoholic solution of oxalic 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. fiber reinforced nylon composite material according to claim 2, which is characterized in that the graphene and the oxalic acid
Mass ratio be 1:2~6, the mass ratio of the graphene and the sodium metaaluminate is 1:3~7.
4. fiber reinforced nylon composite material according to claim 2, which is characterized in that the alcoholic solution is that ethyl alcohol is molten
Liquid, propanol solution or butanol solution.
5. fiber reinforced nylon composite material according to claim 1, which is characterized in that the toughener is selected from maleic acid
At least one of acid anhydride grafted ethene-octene copolymer, glycidyl methacrylate graft ethylene-octene copolymer.
6. fiber reinforced nylon composite material 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. fiber reinforced nylon composite material according to claim 1, which is characterized in that the antioxidant is hindered phenol
At least one of class, thioesters, phosphite ester antioxidant.
8. fiber reinforced nylon composite material according to claim 1, which is characterized in that the lubricant is polyethylene
At least one of wax, stearate, ethylene bis stearamide, grafting ethylene bis stearamide.
9. the preparation method of fiber reinforced nylon composite material as described in claim 1, which is characterized in that including following step
It is rapid:
1) 60~80 parts of nylon66 fiber, 10~20 parts of organosilicon modified polyester acrylate, aramid fiber 5~10 are weighed according to the proportion
Part, 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 anti-oxidant
0.2~0.6 part of agent spare；
2) nylon66 fiber, toughener, aramid 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, 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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| Application Number | Priority Date | Filing Date | Title |
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| CN201810752085.7A CN109082113A (en) | 2018-07-10 | 2018-07-10 | Fiber reinforced nylon composite material and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810752085.7A CN109082113A (en) | 2018-07-10 | 2018-07-10 | Fiber reinforced nylon composite material and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112480652A (en) * | 2020-11-26 | 2021-03-12 | 上海金发科技发展有限公司 | Long glass fiber reinforced TPU/PA alloy material and preparation method thereof |
| CN115559013A (en) * | 2022-03-19 | 2023-01-03 | 福建省天鑫高科新材料有限公司 | Antifouling high-strength graphene nylon long fiber and production process thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104556002A (en) * | 2014-12-19 | 2015-04-29 | 林前锋 | Method for preparing high-purity graphene |
| 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 |
-
2018
- 2018-07-10 CN CN201810752085.7A patent/CN109082113A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104556002A (en) * | 2014-12-19 | 2015-04-29 | 林前锋 | Method for preparing high-purity graphene |
| 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 (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112480652A (en) * | 2020-11-26 | 2021-03-12 | 上海金发科技发展有限公司 | Long glass fiber reinforced TPU/PA alloy material and preparation method thereof |
| CN112480652B (en) * | 2020-11-26 | 2022-12-27 | 金发科技股份有限公司 | Long glass fiber reinforced TPU/PA alloy material and preparation method thereof |
| CN115559013A (en) * | 2022-03-19 | 2023-01-03 | 福建省天鑫高科新材料有限公司 | Antifouling high-strength graphene nylon long fiber and production process thereof |
| CN115559013B (en) * | 2022-03-19 | 2023-12-19 | 福建省天鑫高科新材料有限公司 | Anti-fouling high-strength graphene nylon long fiber and production process thereof |
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