CN108841168A - High temperature resistance high heat conduction nylon composite materials and preparation method thereof - Google Patents
High temperature resistance high heat conduction nylon composite materials and preparation method thereof Download PDFInfo
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- CN108841168A CN108841168A CN201810752084.2A CN201810752084A CN108841168A CN 108841168 A CN108841168 A CN 108841168A CN 201810752084 A CN201810752084 A CN 201810752084A CN 108841168 A CN108841168 A CN 108841168A
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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
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/222—Magnesia, i.e. magnesium oxide
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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
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- 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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Abstract
The invention proposes a kind of high temperature resistance high heat conduction 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 magnesia, 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, pimelic 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 high temperature resistance high heat conduction nylon composite materials 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.
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 high temperature resistance high heat conduction nylon composite materials, 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.
The technical proposal of the invention is realized in this way：
A kind of high temperature resistance high heat conduction nylon composite materials, 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 magnesia, 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, pimelic 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 pimelic 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 pimelic 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 high temperature resistance high heat conduction nylon composite materials, including following
Step：
1) 60~80 parts of nylon, 10~20 parts of organosilicon modified polyester acrylate, magnesia 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) nylon, toughener, magnesia 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：
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 magnesia with
Modified graphene disperses wherein, substantially increases its thermal coefficient and mechanical property.
2, the present invention, can by the modified graphene for selecting mainly to be prepared by graphene, pimelic acid and sodium metaaluminate
To be evenly dispersed into matrix resin very much, so that the interface cohesive force between modified graphene and nylon becomes strong, compatibility is high,
And it is coated on the surface of nylon particle well, forms 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 pimelic 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 pimelic 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 pimelic 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 pimelic acid is 1:2, the mass ratio of graphene and sodium metaaluminate is 1:7.
Embodiment 3
A kind of high temperature resistance high heat conduction nylon composite materials, according to the number of parts by weight, including following raw material：
70 parts of nylon, 14 parts of organosilicon modified polyester acrylate, 7 parts of magnesia, embodiment 1 modified graphene 24
Part, 6 parts of maleic anhydride grafted ethene-octene copolymer, 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 high temperature resistance high heat conduction nylon composite materials：
1) nylon, maleic anhydride grafted ethene-octene copolymer, magnesia 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 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 high temperature resistance high heat conduction nylon composite materials, according to the number of parts by weight, including following raw material：
60 parts of nylon, 20 parts of organosilicon modified polyester acrylate, 5 parts of magnesia, embodiment 2 modified graphene 20
Part, 8 parts of glycidyl methacrylate graft ethylene-octene copolymer, 0.6 part of maleic anhydride grafted polyphenylene ether, ethylene are double
0.2 part of stearmide and 0.2 part of thioesters antioxidant.
The preparation method of high temperature resistance high heat conduction nylon composite materials：
1) changing nylon, glycidyl methacrylate graft ethylene-octene copolymer, magnesia 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 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 high temperature resistance high heat conduction nylon composite materials, according to the number of parts by weight, including following raw material：
0 part of nylon 8,10 parts of organosilicon modified polyester acrylate, 10 parts of magnesia, embodiment 1 modified graphene 30
Part, 4 parts of maleic anhydride grafted ethene-octene copolymer, 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 high temperature resistance high heat conduction nylon composite materials：
1) nylon, maleic anhydride grafted ethene-octene copolymer, magnesia 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 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 high temperature resistance high heat conduction nylon composite materials of embodiment 3-5 are tested for the property, the results are shown in Table 1.
The high temperature resistance high heat conduction 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 high temperature resistance high heat conduction nylon composite materials, which is characterized in that 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 magnesia, 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；It is described
Modified graphene is mainly prepared by graphene, pimelic acid and sodium metaaluminate.
2. high temperature resistance high heat conduction nylon composite materials according to claim 1, which is characterized in that the modified graphene
Preparation method includes can following steps：
1) graphene is added in the alcoholic solution of pimelic 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. high temperature resistance high heat conduction nylon composite materials according to claim 2, which is characterized in that the graphene with it is described
The mass ratio of pimelic acid is 1:2~6, the mass ratio of the graphene and the sodium metaaluminate is 1:3~7.
4. high temperature resistance high heat conduction nylon composite materials according to claim 2, which is characterized in that the alcoholic solution is ethyl alcohol
Solution, propanol solution or butanol solution.
5. high temperature resistance high heat conduction nylon composite materials according to claim 1, which is characterized in that the toughener is selected from horse
At least one in maleic anhydride grafted ethylene-octene copolymer, glycidyl methacrylate graft ethylene-octene copolymer
Kind.
6. high temperature resistance high heat conduction nylon composite materials according to claim 1, which is characterized in that the compatilizer, which is selected from, is
At least one of styrene-maleic anhydride copolymer, maleic anhydride grafted polyphenylene ether.
7. high temperature resistance high heat conduction nylon composite materials according to claim 1, which is characterized in that the antioxidant is to be obstructed
At least one of phenols, thioesters, phosphite ester antioxidant.
8. high temperature resistance high heat conduction nylon composite materials according to claim 1, which is characterized in that the lubricant is poly- second
At least one of alkene wax, stearate, ethylene bis stearamide, grafting ethylene bis stearamide.
9. the preparation method of high temperature resistance high heat conduction nylon composite materials as described in claim 1, which is characterized in that including following
Step：
1) weigh according to the proportion 60~80 parts of nylon, 10~20 parts of organosilicon modified polyester acrylate, 5~10 parts of magnesia,
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 antioxidant
0.2~0.6 part spare；
2) nylon, toughener, magnesia 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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| CN201810752084.2A CN108841168A (en) | 2018-07-10 | 2018-07-10 | High temperature resistance high heat conduction nylon composite materials and preparation method thereof |
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| CN201810752084.2A CN108841168A (en) | 2018-07-10 | 2018-07-10 | High temperature resistance high heat conduction nylon composite materials and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115260942A (en) * | 2022-08-26 | 2022-11-01 | 广东粤辉科技股份有限公司 | Be arranged in car battery can carve sign indicating number and trace back electric core sticky tape |
| CN116285318A (en) * | 2023-04-10 | 2023-06-23 | 中山市乐力隆工程塑料有限公司 | Light heat conduction engineering plastic and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 CN201810752084.2A patent/CN108841168A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
|---|---|---|---|---|
| CN115260942A (en) * | 2022-08-26 | 2022-11-01 | 广东粤辉科技股份有限公司 | Be arranged in car battery can carve sign indicating number and trace back electric core sticky tape |
| CN116285318A (en) * | 2023-04-10 | 2023-06-23 | 中山市乐力隆工程塑料有限公司 | Light heat conduction engineering plastic and preparation method thereof |
| CN116285318B (en) * | 2023-04-10 | 2023-10-27 | 中山市乐力隆工程塑料有限公司 | Light heat conduction engineering plastic and preparation method thereof |
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Application publication date: 20181120 |