CN108276770A - A kind of modified white graphite alkene/polyamide composite heat conducting material and preparation method thereof - Google Patents
A kind of modified white graphite alkene/polyamide composite heat conducting material and preparation method thereof Download PDFInfo
- Publication number
- CN108276770A CN108276770A CN201810012218.7A CN201810012218A CN108276770A CN 108276770 A CN108276770 A CN 108276770A CN 201810012218 A CN201810012218 A CN 201810012218A CN 108276770 A CN108276770 A CN 108276770A
- Authority
- CN
- China
- Prior art keywords
- graphite alkene
- white graphite
- modified
- weight
- conducting material
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
- C08K9/10—Encapsulated ingredients
-
- 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
- C08K3/38—Boron-containing compounds
-
- 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
-
- 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
- C08K3/38—Boron-containing compounds
- C08K2003/382—Boron-containing compounds and nitrogen
- C08K2003/385—Binary compounds of nitrogen with boron
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
The present invention relates to nanocomposite technical fields, and in particular to modified white graphite alkene/polyamide composite heat conducting material and preparation method thereof, Heat Conduction Material includes by weight：80~100 parts of PA resins, modified 0.5~20 part of white graphite alkene, 0.1~3 part of antioxidant, 0.3~3 part of lubricant；The modified white graphite alkene is 2~10 layers of white graphite alkene first after the processing of surface lipophile, then the white graphite alkene that obtains being modified by polymer overmold through in-situ polymerization.It after the mixing in proportion of the material, using double screw extruder melt blending, squeezes out, then tie rod, cooling, air-dried, pelletizing obtains polyamide compoiste material.Modification white graphite alkene/polyamide heat-conducting composite material of preparation has the series of advantages such as high heat conductance, high tenacity, proportion be small, can be widely applied in Lamp cup, lamp holder of LED light etc., to ensure that the good heat dissipation effect of LED light.
Description
Technical field
The present invention relates to Heat Conduction Material technical fields, and in particular to a kind of modified white graphite alkene/polyamide composite heat-conducting material
Material and preparation method thereof.
Background technology
Polyamide is commonly called as nylon (Nylon), and English name Polyamide, abbreviation PA are on molecular backbone containing repetition acyl
The thermoplastic resin general name of amine groups.PA materials because have high intensity, high-wearing feature, good oil resistivity and be widely used in
LED illumination, auto industry and electronic enterprises etc..But PA, as a kind of polymer material, heat conduction and heat radiation ability is general
(thermal conductivity is only 0.25W/ (mK)), therefore limit its application in above-mentioned field.
The method of conventional promotion plastics thermal conductivity is filling heat filling, and existing heat filling includes aluminium nitride, carbon
SiClx, magnesia, silica, aluminium oxide etc., according to thermal conduction mechanism, these heat fillings need to add 40wt% or more could be bright
The aobvious thermal conductivity for promoting composite material, but so the toughness of material and processing performance can be caused to be remarkably decreased under high additive amount.
Invention content
In view of this, it is necessary to which the shortcomings that being directed to existing heat filling provides a kind of machine that PA resins can be kept excellent
Tool performance, and modification white graphite alkene/polyamide composite heat conducting material and preparation method thereof that thermal conductivity can be effectively improved.
To achieve the above object, the present invention takes technical solution below：
The present invention modification white graphite alkene/polyamide composite heat conducting material, include by weight：80~100 parts of PA resins,
Modified 0.5~20 part of white graphite alkene, 0.1~3 part of antioxidant, 0.3~3 part of lubricant；
The modified white graphite alkene is that 2~10 layers of white graphite alkene first obtain after the processing of surface lipophile, then through in-situ polymerization
To the white graphite alkene modified by polymer overmold.
White graphite alkene has high thermal conductivity, high mechanical properties and insulation performance, and it is excellent that a small amount of addition can assign resin
Heat conductivility, while can also improve the impact flexibility of resin, and white graphite alkene is that transparence will not after resin matrix is added
Influence its coloring.
Further, 95 parts of the PA resins, modified 5 parts of white graphite alkene, 1 part of antioxidant, 2 parts of lubricant.
Further, the PA resins include PA6, PA66, PA11, PA12, PA46, PA610, PA1010, in PA612
At least one, preferably PA66.
Further, the antioxidant include four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol esters,
β-(3,5- di-tert-butyl-hydroxy phenyls) propionic acid octadecanols ester, N, N'- is bis--(3- (3,5- di-t-butyl -4- hydroxy benzenes
Base) propiono) hexamethylene diamine, 2,6- di-tert-butyl-4-methy phenols, 4,4'- thiobis (6- tertiary butyl -3- methylphenols), three
The double octadecyl esters of [2.4- di-tert-butyl-phenyls] phosphite ester, pentaerythrite diphosphorous acid, thio-2 acid double octadecyl ester, thio two
At least one of double lauryls of propionic acid；
The lubricant includes calcium stearate, zinc stearate, barium stearate, N,N' ethylene bis stearmide, Ji Wusi
At least one of alcohol stearate.
Further, 300~500m of specific surface area of the modified white graphite alkene2/g.Due to the unique knot of white graphite alkene
Structure and surface energy, for most of oiliness monomers such as styrene, methyl methacrylate etc., when polymerisation, is difficult in white graphite
Alkene material surface is smoothed out, therefore, it is necessary to carry out surface oleophylicization processing to it, monomer can be made to occur on its surface in situ poly-
Conjunction forms clad.
Specifically, the preparation process of the modified white graphite alkene, includes the following steps：
S1, the processing of dialogue graphene surface
The white graphite alkene of 1~20 part of weight is dispersed in the dispersion solution of 100 parts of weight, 0.1~5 part is added after dispersion
The stabilizer of weight is surface-treated；
S2, monomer are in white graphite alkene surface aggregate
White graphite alkene dispersion liquid after S1 is surface-treated is warming up to 60 DEG C~120 DEG C, 1~5 part of weight of addition is drawn
Agent is sent out, stirring keeps solution uniform, and the polymer monomer of 0.1~10 part of weight is then added dropwise, and 0.5~3h is dripped off；After being added dropwise,
Continue after keeping the temperature 30min~2h reactions, adjusts pH value to 7~8, be then rapidly cooled to 20-30 DEG C.
S3, post-processing
The cooled product that will be obtained by S2, washed, filtering, it is dry and grind high polymer cladding white graphite alkene.
The method of the present invention is that dialogue graphene surface carries out after simply handling, and allows monomer to be formed in its surface aggregate and coats
Layer.Present invention modification white graphite alkene preparation method is simple, mild condition, selects suitable initiator, the high polymer cladding of preparation
White graphite alkene coating thickness it is controllable, coating thickness is uniform, and monomer is slowly added dropwise, and cladding process is made orderly to carry out, optimization
Acid-base value after completion of the reaction and temperature condition effectively terminate reaction, obtain best covered effect.The clad of high polymer can be kept away
Exempt to be in direct contact between white graphite alkene, prevents it from reuniting, white graphite alkene and the interface performance of composite substrate can be enhanced, be allowed to
It is dispersed in matrix resin, promotes the formation of entire material system piece layered network, to improve the performance of resin.In addition
Low molecular weight surface-active is can completely avoid to migrate to physical and mechanical property poor processability, surface caused by material surface
The problems such as blistering.
Further, the processing of dialogue graphene surface is in S1：The white graphite alkene of 10~15 parts of weight is dispersed in 100 parts
In the dispersion solution of weight, the stabilizer that 0.1~0.4 part of weight is added after dispersion is modified processing.
Further, surface treatment mode described in S1 is grinding or impregnates.
Further, solution is disperseed described in S1 includes：One or more of water, ethyl alcohol or ethylene glycol etc. mix；Institute
Stating stabilizer includes：It is one or more in polyvinylpyrrolidone, sodium alkyl sulfate, sodium alkyl benzene sulfonate, oleyl amine or oleic acid etc..
Preferably, it is ethyl alcohol to disperse solution described in S1；The stabilizer is oleyl amine or oleic acid.
Further, monomer described in S2 is in white graphite alkene surface aggregate：After the surface treatment of 10~20 parts of weight
White graphite alkene dispersion liquid be warming up to 80 DEG C~90 DEG C, the initiator of 3~5 parts of weight is added, 10~30min of stirring keeps solution equal
It is even, the polymer monomer of 0.5~5 part of weight is added dropwise dropwise, 0.5~1h is dripped off；After being added dropwise, continue heat preservation 1~2h reactions
After complete, pH value is adjusted to 7~8, is then rapidly cooled to 20~30 DEG C.
Further, polymerized monomer described in S2 is：Styrene, acrylic acid, methyl acrylate, ethyl acrylate, propylene
It is one or more in the monomers such as sour hydroxyl ethyl ester, methyl methacrylate, glycidyl methacrylate.
Further, initiator described in S2 is ammonium persulfate or azodiisobutyronitrile.
Further, washing, drying process described in S3, specially use ethanol wash, are done at 60~80 DEG C
It is dry.
A kind of preparation method of modified white graphite alkene/polyamide composite heat conducting material, the specific steps are：By PA resins, resist
Oxygen agent, lubricant are proportionally added into high-speed mixer and are uniformly mixed, then through double screw extruder melt blending, extrusion, then
Tie rod, cooling, air-dried, pelletizing obtain polyamide compoiste material.
Further, the high-speed mixer rotating speed is 1000~3000rpm.
Further, each area's temperature of the double screw extruder be respectively 200~220 DEG C of an area, 220~250 DEG C of 2nd area,
Three 230~260 DEG C of areas, 240~270 DEG C of 4th area, 240~270 DEG C of 5th area, 240~270 DEG C of 6th area, 240~260 DEG C of 7th area, eight
240~260 DEG C of area, 230~250 DEG C of 9th area, 230~260 DEG C of head, vacuum degree >=0.06MPa, engine speed be 300~
500rpm, 30~45Hz of feeding rotating speed.
Further, the double-screw extruder screw diameter can be 35mm, 40mm, 45mm or 50mm, draw ratio
Can be 44：1、40：1 or 30：1.
Beneficial effects of the present invention are：
The white graphite alkene that cement-based powder material coating decoration is modified in the present invention forms good interfacial structure with PA matrixes, makes white
Graphene is realized good evenly dispersed in PA matrixes；Modification white graphite alkene/polyamide heat-conducting composite material of preparation has
The series of advantages such as high heat conductance, high tenacity, proportion is small, can be widely applied in Lamp cup, lamp holder of LED light etc., to protect
The good heat dissipation effect of LED light is demonstrate,proved.
Specific implementation mode
To make the object, technical solutions and advantages of the present invention clearer, below in conjunction with the embodiment of the present invention, to this hair
Bright technical solution work further clearly and completely describes.It should be noted that described embodiment is only the present invention one
Section Example, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not doing
Go out the every other embodiment obtained under the premise of creative work, shall fall within the protection scope of the present invention.
Embodiment 1
The preparation of modified white graphite alkene
It takes 10 parts 2~10 layers of white graphite alkene powder to be added into round-bottomed flask, and 100ml is added into round-bottomed flask and steams
Distilled water, then ultrasonic disperse, 0.2 part of lauryl sodium sulfate is added into round-bottomed flask, and ultrasonic high-speed stirred obtains oleophylic and changes
Property white graphite alkene；
After the white graphite alkene dispersion liquid that 10 parts of oleophylics are modified is heated to 85 DEG C, 1 part of ammonium persulfate initiator, stirring is added
Start that 1 part of methyl methacrylate is added dropwise after 10min, 0.5h is dripped off.After being added dropwise, heat preservation 30min waits for that reaction is completed.Reaction
After to adjust pH value with ammonium hydroxide be 7, be rapidly cooled to room temperature, be filtered under diminished pressure, wine is used after being washed with distilled water filter cake 3~4 times
Essence washed once, and is dried in vacuo at 60 DEG C, and grinding obtains the white graphite alkene of polymethyl methacrylate coating decoration.
Prepare modified white graphite alkene/polyamide composite heat conducting material
By 100 parts of PA66 resins, 4 parts of modified white graphite alkene, 0.1 part of N, N'- be bis--(3- (3,5- di-t-butyl -4- hydroxyls
Phenyl) propiono) hexamethylene diamine, 0.3 part of three [2,4- di-tert-butyl-phenyl] phosphite ester, 0.3 part of N, N'- ethylenebis stearoyls
High-speed mixer is added in amine, is uniformly mixed at 1800rpm, then through double screw extruder melt blending, squeezes out, tie rod is cold
But, it air-dries, pelletizing obtains insulating heat-conductive polyamide compoiste material.Wherein, each area's temperature of extruder is respectively 230 DEG C of an area, two
230 DEG C of area, 250 DEG C of 3rd area, 260 DEG C of 4th area, 270 DEG C of 5th area, 270 DEG C of 6th area, 260 DEG C of 7th area, 260 DEG C of 8th area, nine areas 250
DEG C, 260 DEG C, vacuum degree 0.06MPa, engine speed 380rpm of head, feeding rotating speed 40Hz.
The thermal conductivity that sample is made in test is 3.2W/ (mK), tensile strength 92.5MPa, notch impact strength
8.9KJ/m2。
Embodiment 2
The preparation of modified white graphite alkene
It takes 15 parts 2~10 layers of white graphite alkene powder to be added into round-bottomed flask, and 100ml second is added into round-bottomed flask
Alcohol, then ultrasonic disperse, 0.5 part of lauryl sodium sulfate is added into round-bottomed flask, and ultrasonic high-speed stirred obtains oleophylic modification
White graphite alkene；
After the white graphite alkene dispersion liquid that 15 parts of oleophylics are modified is heated to 90 DEG C, 1 part of ammonium persulfate initiator, stirring is added
Start that 1 part of methyl acrylate is added dropwise after 10min, 0.5h is dripped off.After being added dropwise, heat preservation 45min waits for that reaction is completed.Reaction finishes
It is 7 to adjust pH value with ammonium hydroxide afterwards, is rapidly cooled to room temperature, is filtered under diminished pressure, and is washed with alcohol after being washed with distilled water filter cake 3~4 times
It washs once, and vacuum drying grinding obtains the white graphite alkene of polymethyl acrylate coating decoration at 70 DEG C.
Prepare modified white graphite alkene/polyamide composite heat conducting material
By 100 parts of PA66 resins, 4 parts of modified white graphite alkene, 0.1 part of N, N'- be bis--(3- (3,5- di-t-butyl -4- hydroxyls
Phenyl) propiono) hexamethylene diamine, 0.3 part of three [2.4- di-tert-butyl-phenyls] phosphite ester, 0.3 part of N, N'- ethylenebis stearoyls
High-speed mixer is added in amine, is uniformly mixed at 1800rpm, then through double screw extruder melt blending, squeezes out, tie rod is cold
But, it air-dries, pelletizing obtains insulating heat-conductive polyamide compoiste material.Wherein, each area's temperature of extruder is respectively 230 DEG C of an area, two
230 DEG C of area, 250 DEG C of 3rd area, 260 DEG C of 4th area, 270 DEG C of 5th area, 270 DEG C of 6th area, 260 DEG C of 7th area, 260 DEG C of 8th area, nine areas 250
DEG C, 260 DEG C, vacuum degree 0.06MPa, engine speed 380rpm of head, feeding rotating speed 40Hz.
The thermal conductivity that sample is made in test is 3.0W/ (mK), tensile strength 91.8MPa, notch impact strength
8.2KJ/m2。
Embodiment 3
The preparation of modified white graphite alkene
It takes 20 parts 2-10 layers of white graphite alkene powder to be added into round-bottomed flask, and 100ml third is added into round-bottomed flask
Triol, then ultrasonic disperse, 1 part of oleyl amine is added into round-bottomed flask, and ultrasonic high-speed stirred obtains oleophylic and is modified white graphite alkene；
After the white graphite alkene dispersion liquid that 20 parts of oleophylics are modified is heated to 90 DEG C, 1 part of azodiisobutyronitrile initiator is added,
Start that 5 parts of glycidyl acrylate esters are added dropwise after stirring 10min, 0.5h is dripped off.After being added dropwise, heat preservation 60min waits reacting
It completes.It is 7 to adjust pH value with ammonium hydroxide after completion of the reaction, is rapidly cooled to room temperature, is filtered under diminished pressure, is washed with distilled water filter cake 3~4
It is primary with ethanol wash after secondary, and be dried in vacuo at 90 DEG C, grinding obtains poly (glycidyl methacrylate) coating decoration
White graphite alkene.
Prepare modified white graphite alkene/polyamide composite heat conducting material
By 100 parts of PA66 resins, 4 parts of modified white graphite alkene, 0.1 part of N, N'- be bis--(3- (3,5- di-t-butyl -4- hydroxyls
Phenyl) propiono) hexamethylene diamine, 0.3 part of three [2.4- di-tert-butyl-phenyls] phosphite ester, 0.3 part of N, N'- ethylenebis stearoyls
High-speed mixer is added in amine, is uniformly mixed at 1800rpm, then through double screw extruder melt blending, squeezes out, tie rod is cold
But, it air-dries, pelletizing obtains insulating heat-conductive polyamide compoiste material.Wherein, each area's temperature of extruder is respectively 230 DEG C of an area, two
230 DEG C of area, 250 DEG C of 3rd area, 260 DEG C of 4th area, 270 DEG C of 5th area, 270 DEG C of 6th area, 260 DEG C of 7th area, 260 DEG C of 8th area, nine areas 250
DEG C, 260 DEG C, vacuum degree 0.06MPa, engine speed 380rpm of head, feeding rotating speed 40Hz.
The thermal conductivity that sample is made in test is 3.2W/ (mK), tensile strength 92.4MPa, notch impact strength
9.0KJ/m2。
Comparative example 1
By 100 parts of PA66 resins, 0.1 part of N, N'- be bis--(3- (3,5- di-tert-butyl-hydroxy phenyl) propiono) oneself two
Mixed at high speed is added in amine, 0.3 part of three [2.4- di-tert-butyl-phenyls] phosphite ester, 0.3 part of N, N'- ethylenebisstearamides
Machine is uniformly mixed at 1800rpm, then through double screw extruder melt blending, is squeezed out, tie rod, cooling, is air-dried, pelletizing obtains
To insulating heat-conductive polyamide compoiste material.Wherein, each area's temperature of extruder is respectively 230 DEG C of an area, 230 DEG C of 2nd area, three areas 250
DEG C, 260 DEG C of 4th area, 270 DEG C of 5th area, 270 DEG C of 6th area, 260 DEG C of 7th area, 260 DEG C of 8th area, 250 DEG C of 9th area, 260 DEG C of head, vacuum
Spend 0.06MPa, engine speed 380rpm, feeding rotating speed 40Hz.
The thermal conductivity that sample is made in test is 0.26W/ (mK), tensile strength 80.5MPa, notch impact strength
5.7KJ/m2。
Comparative example 2
By 100 parts of PA66 resins, 4 parts of white graphite alkene, 0.1 part of N, N'- be bis--(3- (3,5- di-tert-butyl-hydroxy phenyl)
Propiono) hexamethylene diamine, 0.3 part of three [2.4- di-tert-butyl-phenyls] phosphite ester, 0.3 part of N, N'- ethylenebisstearamides add
Enter high-speed mixer, be uniformly mixed at 1800rpm, then through double screw extruder melt blending, is squeezed out, tie rod, cooling, wind
Dry, pelletizing obtains insulating heat-conductive polyamide compoiste material.Wherein, each area's temperature of extruder is respectively 230 DEG C of an area, two areas 230
DEG C, 250 DEG C of 3rd area, 260 DEG C of 4th area, 270 DEG C of 5th area, 270 DEG C of 6th area, 260 DEG C of 7th area, 260 DEG C of 8th area, 250 DEG C of 9th area, head
260 DEG C, vacuum degree 0.06MPa, engine speed 380rpm, feeding rotating speed 40Hz.
The thermal conductivity that sample is made in test is 0.63W/ (mK), tensile strength 78.2MPa, notch impact strength
4.9KJ/m2。
Comparative example 3
PH value is 5 after the completion of the differing only in of this comparative example and embodiment 1 is reacted, and naturally cools to room temperature.
Comparative example 4
The addition for differing only in ammonium persulfate initiator of this comparative example and embodiment 1 is 6 parts.
High polymer cladding two-dimensional nano sheet material obtained by embodiment 1-3 is dispersed in alcohol, is not reunited within 10 days；Phase
Comparative example 3-4 occurred to reunite and can not apply in the product at 1 day or so under the conditions of.
Several embodiments of the invention above described embodiment only expresses, the description thereof is more specific and detailed, but simultaneously
Cannot the limitation to the scope of the claims of the present invention therefore be interpreted as.It should be pointed out that for those of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the guarantor of the present invention
Protect range.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (10)
1. a kind of modified white graphite alkene/polyamide composite heat conducting material, which is characterized in that include by weight：PA resins 80~
100 parts, modified 0.5~20 part of white graphite alkene, 0.1~3 part of antioxidant, 0.3~3 part of lubricant；
The white graphite alkene is 2~10 layers of white graphite alkene first after the processing of surface lipophile, then through in-situ polymerization be modified to obtain by
The white graphite alkene of polymer overmold modification.
2. modified white graphite alkene/polyamide composite heat conducting material according to claim 1, which is characterized in that the PA trees
95 parts of fat, modified 5 parts of white graphite alkene, 1 part of antioxidant, 2 parts of lubricant.
3. modified white graphite alkene/polyamide composite heat conducting material according to claim 1, which is characterized in that the antioxygen
Agent includes four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol esters, β-(3,5- di-t-butyl -4- hydroxy benzenes
Base) propionic acid octadecanol ester, N, N'- is bis--(3- (3,5- di-tert-butyl-hydroxy phenyl) propiono) hexamethylene diamine, 2,6 two tertiary fourths
Base -4- methylphenols, 4,4'- thiobis (6- tertiary butyl -3- methylphenols), three [2.4- di-tert-butyl-phenyls] phosphite esters,
At least one of the double octadecyl esters of pentaerythrite diphosphorous acid, the double octadecyl esters of thio-2 acid, the double lauryls of thio-2 acid；
The lubricant includes that calcium stearate, zinc stearate, barium stearate, N,N' ethylene bis stearmide, pentaerythrite are hard
At least one of resin acid ester.
4. modified white graphite alkene/polyamide composite heat conducting material according to claim 1, which is characterized in that the modification
300~500m of specific surface area of white graphite alkene2/g。
5. being modified white graphite alkene/polyamide composite heat conducting material according to any one of claims 1-4, feature exists
In the preparation process of the modified white graphite alkene includes the following steps：
S1, dialogue graphene surface are modified
The white graphite alkene of 1~20 part of weight is dispersed in the dispersion solution of 100 parts of weight, 0.1~5 part of weight is added after dispersion
Stabilizer be surface-treated；
S2, monomer are in white graphite alkene surface aggregate
White graphite alkene dispersion liquid after S1 is surface-treated is warming up to 60 DEG C~120 DEG C, the initiator of 1~5 part of weight is added,
Stirring keeps solution uniform, and the polymer monomer of 0.1~10 part of weight is then added dropwise, and 0.5~3h is dripped off；After being added dropwise, continue
After keeping the temperature 30min~2h reactions, pH value is adjusted to 7~8, is then rapidly cooled to 20~30 DEG C；
S3, post-processing
The cooled product that will be obtained by S2, washed, filtering, it is dry and grind high polymer cladding white graphite alkene.
6. modified white graphite alkene/polyamide composite heat conducting material according to claim 5, which is characterized in that dialogue in S1
Graphene surface is handled：The white graphite alkene of 10~15 parts of weight is dispersed in the dispersion solution of 100 parts of weight, is added after dispersion
The stabilizer for entering 0.1~0.4 part of weight is modified processing.
7. modified white graphite alkene/polyamide composite heat conducting material according to claim 5, which is characterized in that described in S1
Disperseing solution includes：One or more of water, ethyl alcohol or ethylene glycol etc. mix；The stabilizer includes：Polyvinylpyrrolidine
It is one or more in ketone, sodium alkyl sulfate, sodium alkyl benzene sulfonate, oleyl amine or oleic acid.
8. modified white graphite alkene/polyamide composite heat conducting material according to claim 5, which is characterized in that described in S2
Monomer is in white graphite alkene surface aggregate：White graphite alkene dispersion liquid after the surface treatment of 10~20 parts of weight is warming up to 80 DEG C
~90 DEG C, the initiator of 3~5 parts of weight is added, 10~30min of stirring keeps solution uniform, 0.5~5 part of weight is added dropwise dropwise
Polymer monomer, 0.5~1h are dripped off；After being added dropwise, continue after 1~2h of heat preservation reacted, adjusts pH value to 7~8, it is then fast
Speed is cooled to 20-30 DEG C.
9. modified white graphite alkene/polyamide composite heat conducting material according to claim 1, which is characterized in that described in S2
Polymerized monomer is：Styrene, acrylic acid, methyl acrylate, ethyl acrylate, hydroxy-ethyl acrylate, methyl methacrylate, first
It is one or more in base glycidyl acrylate monomer.
10. according to the preparation side of modified white graphite alkene/polyamide composite heat conducting material described in any one of claim 1-9
Method, which is characterized in that the specific steps are：PA resins, antioxidant, lubricant are proportionally added into high-speed mixer and are uniformly mixed,
Then through double screw extruder melt blending, extrusion, then tie rod, cooling, air-dried, pelletizing obtains polyamide compoiste material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810012218.7A CN108276770A (en) | 2018-01-05 | 2018-01-05 | A kind of modified white graphite alkene/polyamide composite heat conducting material and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810012218.7A CN108276770A (en) | 2018-01-05 | 2018-01-05 | A kind of modified white graphite alkene/polyamide composite heat conducting material and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108276770A true CN108276770A (en) | 2018-07-13 |
Family
ID=62803349
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810012218.7A Pending CN108276770A (en) | 2018-01-05 | 2018-01-05 | A kind of modified white graphite alkene/polyamide composite heat conducting material and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108276770A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109850885A (en) * | 2019-02-19 | 2019-06-07 | 广东烯王科技有限公司 | One kind clicking addition chemical modification white graphite alkene and preparation method thereof based on sulfydryl-alkene |
| CN109880169A (en) * | 2019-01-08 | 2019-06-14 | 常州兴烯石墨烯科技有限公司 | Modified white graphite alkene nylon compound slice of a kind of in-situ polymerization and preparation method thereof |
| CN109880353A (en) * | 2019-02-19 | 2019-06-14 | 广东烯王科技有限公司 | A kind of white graphite alkene composite polyamide material, film and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102786815A (en) * | 2012-08-15 | 2012-11-21 | 中国科学院上海硅酸盐研究所 | Method for modifying surface of BN (boron nitride) powder, modified BN and polymer composite material |
| CN104927330A (en) * | 2015-06-15 | 2015-09-23 | 四川大学 | High thermal conductive and insulating polymer composite and preparing method and application thereof |
| CN105175654A (en) * | 2015-09-29 | 2015-12-23 | 中国航空工业集团公司北京航空材料研究院 | Hexagonal boron nitride micro-constrained acrylate latex nanocomposite |
| CN105860315A (en) * | 2016-06-14 | 2016-08-17 | 辽宁大学 | Preparing method of hexagonal boron nitride/polystyrene composite |
| CN106674603A (en) * | 2016-12-29 | 2017-05-17 | 中国科学院深圳先进技术研究院 | Heat-conducting hexagonal boron nitride hybrid material as well as preparation method and application thereof |
-
2018
- 2018-01-05 CN CN201810012218.7A patent/CN108276770A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102786815A (en) * | 2012-08-15 | 2012-11-21 | 中国科学院上海硅酸盐研究所 | Method for modifying surface of BN (boron nitride) powder, modified BN and polymer composite material |
| CN104927330A (en) * | 2015-06-15 | 2015-09-23 | 四川大学 | High thermal conductive and insulating polymer composite and preparing method and application thereof |
| CN105175654A (en) * | 2015-09-29 | 2015-12-23 | 中国航空工业集团公司北京航空材料研究院 | Hexagonal boron nitride micro-constrained acrylate latex nanocomposite |
| CN105860315A (en) * | 2016-06-14 | 2016-08-17 | 辽宁大学 | Preparing method of hexagonal boron nitride/polystyrene composite |
| CN106674603A (en) * | 2016-12-29 | 2017-05-17 | 中国科学院深圳先进技术研究院 | Heat-conducting hexagonal boron nitride hybrid material as well as preparation method and application thereof |
Non-Patent Citations (1)
| Title |
|---|
| 周文英 丁小卫: "《导热高分子材料》", 30 April 2014, 国防工业出版社 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109880169A (en) * | 2019-01-08 | 2019-06-14 | 常州兴烯石墨烯科技有限公司 | Modified white graphite alkene nylon compound slice of a kind of in-situ polymerization and preparation method thereof |
| CN109880169B (en) * | 2019-01-08 | 2021-04-27 | 常州兴烯石墨烯科技有限公司 | In-situ polymerization modified white graphene nylon composite slice and preparation method thereof |
| CN109850885A (en) * | 2019-02-19 | 2019-06-07 | 广东烯王科技有限公司 | One kind clicking addition chemical modification white graphite alkene and preparation method thereof based on sulfydryl-alkene |
| CN109880353A (en) * | 2019-02-19 | 2019-06-14 | 广东烯王科技有限公司 | A kind of white graphite alkene composite polyamide material, film and preparation method thereof |
| CN109880353B (en) * | 2019-02-19 | 2021-07-06 | 广东烯王科技有限公司 | White graphene composite polyamide material, film and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104151706B (en) | Polypropylene composite material and preparation method thereof | |
| CN108276770A (en) | A kind of modified white graphite alkene/polyamide composite heat conducting material and preparation method thereof | |
| CN108047569A (en) | A kind of functional composite material and preparation method thereof | |
| CN103897241A (en) | Heat conductive plastics and manufacturing method thereof | |
| CN103756298B (en) | A kind of thermoplastic polymer based thermal conductive composite and its preparation method and application | |
| CN108165003A (en) | A kind of high content of glass fiber enhancing high-temperature nylon composite material and preparation method thereof | |
| CN102604328A (en) | Matrix resin composition of resin-based fabric reinforced composite mandrel for overhead wire and application method of the resin composition | |
| CN104356585A (en) | High-performance continuous carbon fiber reinforced ABS composite material and preparation method thereof | |
| CN105885222A (en) | Compound polypropylene tubular product production process | |
| CN105566898A (en) | Nano nylon 6 composite material | |
| CN106554553A (en) | Easy processing metallocene PE compositionss and preparation method thereof | |
| CN105542449A (en) | Preparation method of nylon 6 nanocomposite material | |
| CN108017820A (en) | A kind of fiber reinforcement high density polyethylene (HDPE)/graphene composite material and preparation method thereof | |
| CN102936410B (en) | A kind of in-situ polymerization prepares the method for polyamide-based heat-conductive composite material | |
| CN106751173A (en) | The pvc material and manufacture method of a kind of Wear-resistant, high-temperature resistant | |
| CN1256378C (en) | Method for preparing nano composite material of polyethylene/montmorillonite | |
| CN104559146A (en) | Whisker reinforced thermally conductive plastic material and preparation method thereof | |
| CN104371229A (en) | High-wettability and high-strength continuous carbon fiber reinforced polyvinylidene fluoride (PVDF) composite material and preparation method thereof | |
| CN102002229A (en) | Long fiber reinforced nylon composite material and preparation method thereof | |
| CN107815054A (en) | A kind of PA composites and preparation method thereof with low water absorption, strong thermal conductivity | |
| CN108503972A (en) | Composite polyethylene material and preparation method thereof | |
| CN105153631B (en) | A kind of coating modified fibre reinforced ABS resin composite material and preparation method | |
| CN105907024A (en) | Low-cost fiber-reinforced ABS wood-plastic composite and preparation method thereof | |
| CN106349689B (en) | Toughening enhances PA6 materials and preparation method thereof | |
| CN108299681A (en) | A kind of method of high polymer cladding two-dimensional nano sheet material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180713 |
|
| RJ01 | Rejection of invention patent application after publication |