CN117362998A - Heat-conducting polymer material and preparation method thereof - Google Patents
Heat-conducting polymer material and preparation method thereof Download PDFInfo
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- CN117362998A CN117362998A CN202311476916.XA CN202311476916A CN117362998A CN 117362998 A CN117362998 A CN 117362998A CN 202311476916 A CN202311476916 A CN 202311476916A CN 117362998 A CN117362998 A CN 117362998A
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- 239000000463 material Substances 0.000 title claims abstract description 38
- 229920001940 conductive polymer Polymers 0.000 title claims abstract description 37
- 239000002322 conducting polymer Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 96
- 229920002292 Nylon 6 Polymers 0.000 claims abstract description 91
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims abstract description 51
- 238000002156 mixing Methods 0.000 claims abstract description 38
- 239000000243 solution Substances 0.000 claims abstract description 24
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 20
- 230000007062 hydrolysis Effects 0.000 claims abstract description 20
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 20
- XHXFXVLFKHQFAL-UHFFFAOYSA-N phosphoryl trichloride Chemical compound ClP(Cl)(Cl)=O XHXFXVLFKHQFAL-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000000843 powder Substances 0.000 claims abstract description 20
- 239000011259 mixed solution Substances 0.000 claims abstract description 13
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 13
- 229920002545 silicone oil Polymers 0.000 claims abstract description 12
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims abstract description 12
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 claims abstract description 11
- CBCKQZAAMUWICA-UHFFFAOYSA-N 1,4-phenylenediamine Chemical compound NC1=CC=C(N)C=C1 CBCKQZAAMUWICA-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000004594 Masterbatch (MB) Substances 0.000 claims abstract description 10
- 238000000227 grinding Methods 0.000 claims abstract description 10
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000002861 polymer material Substances 0.000 claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 66
- 238000003756 stirring Methods 0.000 claims description 47
- 238000001035 drying Methods 0.000 claims description 44
- 238000001914 filtration Methods 0.000 claims description 36
- 238000005406 washing Methods 0.000 claims description 36
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 18
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 18
- 238000006243 chemical reaction Methods 0.000 claims description 16
- 238000001816 cooling Methods 0.000 claims description 16
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- -1 polytetrafluoroethylene Polymers 0.000 claims description 11
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 10
- 235000019441 ethanol Nutrition 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 9
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 9
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 9
- 239000002253 acid Substances 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 238000010992 reflux Methods 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 239000013078 crystal Substances 0.000 claims description 2
- 230000003301 hydrolyzing effect Effects 0.000 claims description 2
- 238000007781 pre-processing Methods 0.000 abstract description 2
- 238000001746 injection moulding Methods 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 22
- 238000012360 testing method Methods 0.000 description 13
- 239000002131 composite material Substances 0.000 description 11
- 238000005457 optimization Methods 0.000 description 8
- 238000005452 bending Methods 0.000 description 6
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 239000003063 flame retardant Substances 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 3
- PEEHTFAAVSWFBL-UHFFFAOYSA-N Maleimide Chemical compound O=C1NC(=O)C=C1 PEEHTFAAVSWFBL-UHFFFAOYSA-N 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000017525 heat dissipation Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 238000004377 microelectronic Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 229920002627 poly(phosphazenes) Polymers 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 206010063385 Intellectualisation Diseases 0.000 description 1
- 239000004677 Nylon Substances 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000011231 conductive filler Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000001066 destructive effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004100 electronic packaging Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000006459 hydrosilylation reaction Methods 0.000 description 1
- 125000004029 hydroxymethyl group Chemical group [H]OC([H])([H])* 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 125000005439 maleimidyl group Chemical group C1(C=CC(N1*)=O)=O 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 229920013657 polymer matrix composite Polymers 0.000 description 1
- 239000011160 polymer matrix composite Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
Classifications
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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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/08—Oxygen-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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- 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)
Abstract
The invention discloses a heat-conducting polymer material and a preparation method thereof, and relates to the field of polymer materials. When the heat-conducting high polymer material is prepared, firstly, a silane coupling agent hydrolysis solution is used for preprocessing the nano alumina whisker, and then the preprocessed nano alumina whisker, p-phenylenediamine and phosphorus oxychloride react to prepare a pre-modified nano alumina whisker; reacting maleic anhydride with the pre-modified nano alumina whisker to obtain the modified nano alumina whisker; grinding the nylon 6 master batch into powder, treating with formaldehyde alkaline mixed solution, and then sequentially reacting with trimethoxysilane and vinyl silicone oil to obtain modified nylon 6; and mixing the modified nano aluminum oxide whisker and the modified nylon 6, extruding, injection molding and demolding to prepare the heat-conducting polymer material. The heat-conducting polymer material prepared by the invention has excellent high temperature resistance, heat conduction and mechanical properties.
Description
Technical Field
The invention relates to the field of high polymer materials, in particular to a heat conduction high polymer material and a preparation method thereof.
Background
With the development of modern electronic components toward integration, miniaturization and intellectualization, the heat dissipation problem of electronic equipment becomes a bottleneck which hinders the development of the microelectronic field, how to timely discharge the heat generated by the electronic components has become an important research topic in the microelectronic product system assembly field, and the general solution is to introduce a heat conducting composite material between the electronic components and the heat dissipation device, so that the polymer matrix composite material has been widely paid attention to because of the advantages of light weight, good insulation, high mechanical strength, low cost and the like.
However, the amorphous structure and vibration of the macromolecular chains result in very low thermal conductivity of most pure polymers themselves, severely restricting their application in the field of thermal interfaces. Therefore, the preparation of polymer-based thermally conductive composites with excellent overall properties by adding highly thermally conductive fillers is a hot spot of current research. However, the current polymer-based heat-conducting composite material still faces the problems of low heat conductivity, large filling amount, unstable performance, high cost and the like, and is difficult to adapt to diversified requirements. Therefore, it is necessary to modify these polymer materials for electronic packaging to increase heat conductive and heat resistant properties and mechanical strength thereof.
Disclosure of Invention
The invention aims to provide a heat-conducting polymer material and a preparation method thereof, which are used for solving the problems in the prior art.
In order to solve the technical problems, the invention provides the following technical scheme:
a heat conducting polymer material mainly comprises: mainly comprises the following steps: modified nano alumina whisker, modified nylon 6 and potassium persulfate.
As optimization, the modified nano alumina whisker is prepared by pretreating the nano alumina whisker by using a silane coupling agent hydrolysis solution, then reacting with p-phenylenediamine and phosphorus oxychloride, and then reacting with maleic anhydride.
As optimization, the modified nylon 6 is prepared by grinding nylon 6 master batches into powder by a pulverizer, treating the powder by formaldehyde alkaline mixed solution, reacting the powder with trimethoxysilane, and reacting the powder with vinyl silicone oil.
The silane coupling agent hydrolysis solution is prepared by hydrolyzing aminopropyl triethoxysilane in ethanol solution with the mass fraction of 70-80%. .
The formaldehyde alkaline mixed solution used for optimization is prepared from sodium hydroxide and formaldehyde aqueous solution with the mass fraction of 10%.
The preparation method of the heat conducting polymer material comprises the following preparation steps:
(1) Mixing aminopropyl triethoxysilane and ethanol with the mass fraction of 70-80% according to the mass ratio of 1:30-40, and stirring at the temperature of 45-55 ℃ for 30-40 min at the speed of 200-300 r/min to obtain a silane coupling agent hydrolysis solution; mixing nano alumina whisker and silane coupling agent hydrolysis solution according to a mass ratio of 1:40-50, stirring for 5-7 h at a temperature of 80-90 ℃ at a speed of 200-300 r/min, filtering, washing for 3-5 times by absolute ethyl alcohol, and drying for 3-5 h at a temperature of 80-90 ℃ to obtain pretreated nano alumina whisker; uniformly mixing the pretreated nano alumina whisker, p-phenylenediamine, phosphorus oxychloride, triethylamine and chloroform according to the mass ratio of 1:10-12:15-18:15-18:150-200 at the temperature of 0-5 ℃ and the speed of 200-300 r/min for 20-30 min, stirring at the temperature of 50-60 ℃ and the speed of 200-300 r/min for reacting for 5-7 h, filtering, respectively washing for 3-5 times by pure water and absolute ethyl alcohol, and drying at the temperature of 75-85 ℃ for 10-14 h to obtain the pre-modified nano alumina whisker; uniformly mixing maleic anhydride, N-dimethylformamide, pre-modified nano alumina whisker and toluene according to a mass ratio of 1:5-6:6-7:100-120, stirring and refluxing for 6-8 hours at a temperature of between 40 and 50 ℃ at a speed of between 200 and 300r/min, filtering, washing for 3 to 5 times by using absolute ethyl alcohol, and drying for 5 to 6 hours at a temperature of between 30 and 40 ℃ to obtain the modified nano alumina whisker;
(2) Grinding the nylon 6 master batch into powder with the particle size smaller than 100 mu m by a pulverizer, immersing the powder into formaldehyde alkaline mixed solution, stirring for 2-3 hours at 80-90 ℃ and 200-300 r/min, filtering, washing for 3-5 times by pure water, and drying for 5-6 hours at 50-60 ℃ to obtain pretreated nylon 6; stirring pretreated nylon 6, trimethoxysilane and absolute ethyl alcohol according to the mass ratio of 1:5-6:20-25 at 50-60 ℃ for reaction for 3-5 hours at 200-300 r/min, filtering, washing with absolute ethyl alcohol for 3-5 times, and drying at 50-60 ℃ for 5-6 hours to obtain the pre-modified nylon 6; mixing the pre-modified nylon 6, vinyl silicone oil and chloroplatinic acid according to the mass ratio of 1:12-13:0.001-0.002, stirring at the temperature of 100-120 ℃ for reaction for 6-8 hours at the speed of 200-300 r/min, filtering, washing with absolute ethyl alcohol for 3-5 times, and drying at the temperature of 50-60 ℃ for 5-6 hours to obtain modified nylon 6;
(3) Drying the modified nano alumina whisker and the modified nylon 6 at 75-85 ℃ for 10-12 hours respectively, uniformly mixing the modified nano alumina whisker, the modified nylon 6 and the potassium persulfate according to the mass ratio of 1-2:10-13:0.01-0.02, extruding and injecting the mixture into a polytetrafluoroethylene template at 250-300 r/min by a double screw extruder at 280-320 ℃, cooling to 80-90 ℃ and preserving heat for 20-24 hours, naturally cooling to room temperature, and demoulding and taking out to obtain the heat conducting polymer material.
As optimization, the reaction process of the modified nano alumina whisker in the step (1) is as follows:
as optimization, the reaction process of the modified nylon 6 in the step (2) is as follows:
as optimization, the purity of the nano alumina whisker in the step (1) is more than 99.9%, and the nano alumina whisker is in a hexagonal crystal form.
As optimization, the preparation method of the silane coupling agent hydrolysis solution in the step (1) comprises the following steps: mixing aminopropyl triethoxysilane and 70-80% ethanol according to a mass ratio of 5:150-180, and stirring at 45-55 ℃ for 30-40 min at 200-300 r/min.
As optimization, the preparation method of the formaldehyde alkaline mixed solution in the step (2) comprises the following steps: the aqueous solution of sodium hydroxide and formaldehyde with the mass fraction of 10 percent is stirred for 30 to 40 minutes at the room temperature with the mass ratio of 200 to 300r/min according to the mass ratio of 1:45 to 55.
Compared with the prior art, the invention has the following beneficial effects:
when the heat-conducting polymer material is prepared, the modified nano aluminum oxide whisker and the modified nylon 6 are uniformly mixed, extruded and injected into a polytetrafluoroethylene die by a double-screw extruder, and cooled to room temperature, so that the heat-conducting polymer material is prepared.
Firstly, a silane coupling agent hydrolysis solution is used for preprocessing nano aluminum oxide whiskers, amino groups are grafted on the nano aluminum oxide whiskers, so that the dispersibility of the nano aluminum oxide whiskers is improved, meanwhile, the nano aluminum oxide whiskers react with p-phenylenediamine and phosphorus oxychloride to generate a polyphosphazene hyperbranched chain, wherein the content of flame retardant elements such as nitrogen and phosphorus is high, a nitrogen and phosphorus flame retardant synergistic flame retardant system can be formed, the material has good flame retardant effect, and the formed crosslinked network can improve the mechanical strength of the material; then reacts with maleic anhydride to form a maleimide structure at the edge of the cross-linked network, so that the heat resistance of the network can be effectively improved, the compatibility of the nano aluminum oxide whisker and nylon 6 can be improved, and the interface heat resistance can be effectively reduced, thereby improving the heat conductivity.
Secondly, grinding the nylon 6 master batch into powder, then treating the powder with formaldehyde alkaline mixed solution to generate hydroxymethyl active groups on the surface of the nylon 6, then reacting with trimethoxysilane, grafting trimethoxysilane on the surface of the nylon 6 to obtain pre-modified nylon 6, and grafting vinyl silicone oil on the nylon 6 through hydrosilylation of the pre-modified nylon 6, vinyl silicone oil and chloroplatinic acid, thereby forming a polyvinyl polysiloxane structure on the surface of the nylon 6.
And finally, mixing and heating the modified nylon 6, the modified nano aluminum oxide whisker and potassium persulfate to polymerize a large number of double bonds on the polysiloxane structure of the modified nylon 6 and the double bonds of maleimide on the hyperbranched network edge of the nano aluminum oxide whisker under the catalysis of potassium persulfate, so that a crosslinked network is formed, the compatibility is improved, the interface thermal resistance is reduced, the thermal conductivity is improved, and the mechanical property and the heat-resistant stability of the material are improved.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The preparation method of the heat-conducting polymer material comprises the following preparation steps:
(1) Mixing aminopropyl triethoxysilane and 70% ethanol according to a mass ratio of 5:150, and stirring at 45 ℃ for 40min at 200r/min to obtain a silane coupling agent hydrolysis solution; mixing nano alumina whisker and a silane coupling agent hydrolysis solution according to a mass ratio of 1:40, stirring at 80 ℃ for 7 hours at 200r/min, filtering, washing with absolute ethyl alcohol for 3 times, and drying at 80 ℃ for 5 hours to obtain pretreated nano alumina whisker; uniformly mixing the pretreated nano alumina whisker, p-phenylenediamine, phosphorus oxychloride, triethylamine and chloroform according to the mass ratio of 1:10:15:15:150 at 0 ℃ and stirring at 200r/min for 30min, reacting at 50 ℃ and stirring at 200r/min for 7h, filtering, respectively washing for 3 times by using pure water and absolute ethyl alcohol, and drying at 75 ℃ for 14h to obtain the pre-modified nano alumina whisker; stirring and refluxing maleic anhydride, N-dimethylformamide, pre-modified nano alumina whiskers and toluene at a mass ratio of 1:5:6:100 at a temperature of 200r/min for 8 hours, filtering, washing with absolute ethyl alcohol for 3 times, and drying at a temperature of 30 ℃ for 6 hours to obtain modified nano alumina whiskers;
(2) Grinding nylon 6 master batch into powder with the particle size smaller than 100 mu m by a pulverizer, immersing the powder into formaldehyde alkaline mixed solution, stirring for 3 hours at 80 ℃ for 200r/min, filtering, washing for 3 times by pure water, and drying for 5 hours at 50 ℃ to obtain pretreated nylon 6; stirring pretreated nylon 6, trimethoxysilane and absolute ethyl alcohol according to the mass ratio of 1:5:20 at 50 ℃ for reaction for 5 hours at 200r/min, filtering, washing with absolute ethyl alcohol for 3 times, and drying at 50 ℃ for 6 hours to obtain pre-modified nylon 6; mixing pre-modified nylon 6, vinyl silicone oil and chloroplatinic acid according to the mass ratio of 1:12:0.001, stirring at 100 ℃ for reaction for 8 hours at 200r/min, filtering, washing with absolute ethyl alcohol for 3 times, and drying at 50 ℃ for 6 hours to obtain modified nylon;
(3) Drying modified nano alumina whisker and modified nylon 6 at 75 ℃ for 12 hours respectively, uniformly mixing the modified nano alumina whisker, the modified nylon 6 and potassium persulfate according to a mass ratio of 1:10:0.01, extruding and injecting the mixture into a polytetrafluoroethylene template at 280 ℃ by a double screw extruder at 250r/min, cooling to 80 ℃ and preserving heat for 24 hours, naturally cooling to room temperature, and demoulding and taking out to obtain the heat-conducting polymer material.
Example 2
The preparation method of the heat-conducting polymer material comprises the following preparation steps:
(1) Mixing aminopropyl triethoxysilane and ethanol with the mass fraction of 75% according to the mass ratio of 5:160, and stirring at 50 ℃ for 35min at the speed of 250r/min to obtain a silane coupling agent hydrolysis solution; mixing nano alumina whisker and silane coupling agent hydrolysis solution according to a mass ratio of 1:45, stirring at a temperature of 85 ℃ for 6 hours at a speed of 250r/min, filtering, washing with absolute ethyl alcohol for 4 times, and drying at a temperature of 85 ℃ for 4 hours to obtain pretreated nano alumina whisker; uniformly mixing the pretreated nano aluminum oxide whisker, p-phenylenediamine, phosphorus oxychloride, triethylamine and chloroform according to the mass ratio of 1:11:16.5:16.5:175 at 2.5 ℃ at 250r/min for 25min, stirring at 55 ℃ at 250r/min for reaction for 6h, filtering, respectively washing for 4 times by using pure water and absolute ethyl alcohol, and drying at 80 ℃ for 12h to obtain the pre-modified nano aluminum oxide whisker; stirring and refluxing maleic anhydride, N-dimethylformamide, pre-modified nano alumina whiskers and toluene at the mass ratio of 1:5.5:6.5:110 at the temperature of 45 ℃ for 7 hours at the speed of 250r/min, filtering, washing with absolute ethyl alcohol for 4 times, and drying at the temperature of 35 ℃ for 5.5 hours to obtain modified nano alumina whiskers;
(2) Grinding nylon 6 master batch into powder with the particle size smaller than 100 mu m by a pulverizer, immersing the powder into formaldehyde alkaline mixed solution, stirring at 85 ℃ and 250r/min for 2.5 hours, filtering, washing with pure water for 4 times, and drying at 5 ℃ for 5.5 hours to obtain pretreated nylon 6; stirring pretreated nylon 6, trimethoxysilane and absolute ethyl alcohol according to the mass ratio of 1:5.5:22.5 at the temperature of 55 ℃ for reaction for 4 hours at the speed of 250r/min, filtering, washing with absolute ethyl alcohol for 4 times, and drying at the temperature of 55 ℃ for 5.5 hours to obtain pre-modified nylon 6; mixing the pre-modified nylon 6, vinyl silicone oil and chloroplatinic acid according to the mass ratio of 1:12.5:0.0015, stirring at the temperature of 110 ℃ for reaction for 7 hours at the speed of 250r/min, filtering, washing with absolute ethyl alcohol for 4 times, and drying at the temperature of 55 ℃ for 5.5 hours to obtain modified nylon 6;
(3) Drying the modified nano alumina whisker and the modified nylon 6 at 80 ℃ for 11 hours respectively, uniformly mixing the modified nano alumina whisker, the modified nylon 6 and the potassium persulfate according to the mass ratio of 1.5:12:0.015, extruding and injecting the mixture into a polytetrafluoroethylene template at 275r/min by using a double-screw extruder at 300 ℃, cooling to 85 ℃, preserving heat for 22 hours, naturally cooling to room temperature, and demoulding and taking out to obtain the heat-conducting polymer material.
Example 3
The preparation method of the heat-conducting polymer material comprises the following preparation steps:
(1) Mixing aminopropyl triethoxysilane and 80% ethanol according to a mass ratio of 5:180, and stirring at 55 ℃ for 30min at 300r/min to obtain a silane coupling agent hydrolysis solution; mixing nano alumina whisker and silane coupling agent hydrolysis solution according to a mass ratio of 1:50, stirring at 90 ℃ for 5 hours at 300r/min, filtering, washing with absolute ethyl alcohol for 5 times, and drying at 90 ℃ for 3 hours to obtain pretreated nano alumina whisker; uniformly mixing the pretreated nano alumina whisker, p-phenylenediamine, phosphorus oxychloride, triethylamine and chloroform according to the mass ratio of 1:12:18:18:200 at the temperature of 5 ℃ and stirring at the speed of 300r/min for 20min, reacting at the temperature of 60 ℃ and stirring at the speed of 300r/min for 5h, filtering, respectively washing for 5 times by using pure water and absolute ethyl alcohol, and drying at the temperature of 85 ℃ for 10h to obtain the pre-modified nano alumina whisker; stirring and refluxing maleic anhydride, N-dimethylformamide, pre-modified nano alumina whiskers and toluene at the mass ratio of 1:6:7:120 at the temperature of 50 ℃ for 6 hours at the speed of 300r/min, filtering, washing with absolute ethyl alcohol for 5 times, and drying at the temperature of 40 ℃ for 5 hours to obtain modified nano alumina whiskers;
(2) Grinding nylon 6 master batch into powder with the particle size smaller than 100 mu m by a pulverizer, immersing the powder into formaldehyde alkaline mixed solution, stirring for 2 hours at 90 ℃ and 300r/min, filtering, washing for 5 times by pure water, and drying for 5 hours at 60 ℃ to obtain pretreated nylon 6; stirring pretreated nylon 6, trimethoxysilane and absolute ethyl alcohol according to a mass ratio of 1:6:25 at a temperature of 300r/min for reaction for 3 hours, filtering, washing with absolute ethyl alcohol for 5 times, and drying at a temperature of 60 ℃ for 5 hours to obtain pre-modified nylon 6; mixing the pre-modified nylon 6, vinyl silicone oil and chloroplatinic acid according to the mass ratio of 1:13:0.002, stirring at 120 ℃ for reaction for 6 hours at 300r/min, filtering, washing with absolute ethyl alcohol for 5 times, and drying at 60 ℃ for 5 hours to obtain modified nylon 6;
(3) Drying the modified nano alumina whisker and the modified nylon 6 at 85 ℃ for 10 hours respectively, uniformly mixing the modified nano alumina whisker, the modified nylon 6 and the potassium persulfate according to a mass ratio of 2:13:0.02, extruding and injecting the mixture into a polytetrafluoroethylene template at 320 ℃ by a double screw extruder at 300r/min, cooling to 90 ℃ and preserving heat for 20 hours, naturally cooling to room temperature, and demoulding and taking out to obtain the heat-conducting polymer material.
Comparative example 1
The preparation method of the heat-conducting polymer material comprises the following preparation steps:
(1) Grinding nylon 6 master batch into powder with the particle size smaller than 100 mu m by a pulverizer, immersing the powder into formaldehyde alkaline mixed solution, stirring at 85 ℃ and 250r/min for 2.5 hours, filtering, washing with pure water for 4 times, and drying at 5 ℃ for 5.5 hours to obtain pretreated nylon 6; stirring pretreated nylon 6, trimethoxysilane and absolute ethyl alcohol according to the mass ratio of 1:5.5:22.5 at the temperature of 55 ℃ for reaction for 4 hours at the speed of 250r/min, filtering, washing with absolute ethyl alcohol for 4 times, and drying at the temperature of 55 ℃ for 5.5 hours to obtain pre-modified nylon 6; mixing the pre-modified nylon 6, vinyl silicone oil and chloroplatinic acid according to the mass ratio of 1:12.5:0.0015, stirring at the temperature of 110 ℃ for reaction for 7 hours at the speed of 250r/min, filtering, washing with absolute ethyl alcohol for 4 times, and drying at the temperature of 55 ℃ for 5.5 hours to obtain modified nylon 6;
(2) Drying the nano aluminum oxide whisker and the modified nylon 6 at 80 ℃ for 11 hours respectively, uniformly mixing the nano aluminum oxide whisker, the modified nylon 6 and the potassium persulfate according to the mass ratio of 1.5:12:0.015, extruding and injecting the mixture into a polytetrafluoroethylene template at 275r/min by using a double-screw extruder at 300 ℃, cooling to 85 ℃, preserving heat for 22 hours, naturally cooling to room temperature, and demoulding and taking out to obtain the heat-conducting polymer material.
Comparative example 2
The preparation method of the heat-conducting polymer material comprises the following preparation steps:
(1) Mixing aminopropyl triethoxysilane and ethanol with the mass fraction of 75% according to the mass ratio of 5:160, and stirring at 50 ℃ for 35min at the speed of 250r/min to obtain a silane coupling agent hydrolysis solution; mixing nano alumina whisker and silane coupling agent hydrolysis solution according to a mass ratio of 1:45, stirring at a temperature of 85 ℃ for 6 hours at a speed of 250r/min, filtering, washing with absolute ethyl alcohol for 4 times, and drying at a temperature of 85 ℃ for 4 hours to obtain pretreated nano alumina whisker; uniformly mixing the pretreated nano aluminum oxide whisker, p-phenylenediamine, phosphorus oxychloride, triethylamine and chloroform according to the mass ratio of 1:11:16.5:16.5:175 at 2.5 ℃ at 250r/min for 25min, stirring at 55 ℃ at 250r/min for reaction for 6h, filtering, respectively washing for 4 times by using pure water and absolute ethyl alcohol, and drying at 80 ℃ for 12h to obtain the pre-modified nano aluminum oxide whisker; stirring and refluxing maleic anhydride, N-dimethylformamide, pre-modified nano alumina whiskers and toluene at the mass ratio of 1:5.5:6.5:110 at the temperature of 45 ℃ for 7 hours at the speed of 250r/min, filtering, washing with absolute ethyl alcohol for 4 times, and drying at the temperature of 35 ℃ for 5.5 hours to obtain modified nano alumina whiskers;
(2) Drying the modified nano aluminum oxide whisker and nylon 6 at 80 ℃ for 11 hours respectively, uniformly mixing the modified nano aluminum oxide whisker, nylon 6 and potassium persulfate according to the mass ratio of 1.5:12:0.015, extruding and injecting the mixture into a polytetrafluoroethylene template at 275r/min by using a double-screw extruder at 300 ℃, cooling to 85 ℃, preserving heat for 22 hours, naturally cooling to room temperature, and demoulding and taking out to obtain the heat-conducting polymer material.
Comparative example 3
The preparation method of the heat-conducting polymer material comprises the following preparation steps:
drying the nano aluminum oxide whisker and nylon 6 at 80 ℃ for 11 hours respectively, uniformly mixing the nano aluminum oxide whisker, nylon 6 and potassium persulfate according to the mass ratio of 1.5:12:0.015, extruding and injecting the mixture into a polytetrafluoroethylene template at 275r/min by using a double-screw extruder at 300 ℃, cooling to 85 ℃, preserving heat for 22 hours, naturally cooling to room temperature, demoulding and taking out to obtain the heat-conducting polymer material.
Test example 1
Testing of thermal conductivity
The testing method comprises the following steps: the thermal conductivity of the composite material was tested according to the ISO 22007-2.2 standard and measured using a thermal conductivity meter based on the hot wire method. The results are shown in Table 1.
TABLE 1
| Sample of | Thermal conductivity/(W/mK) | Sample of | Thermal conductivity/(W/mK) |
| Example 1 | 0.957 | Comparative example 1 | 0.468 |
| Example 2 | 0.954 | Comparative example 2 | 0.918 |
| Example 3 | 0.963 | Comparative example 3 | 0.427 |
From comparison of experimental data of examples 1 to 3 and comparative examples 1 to 3 in Table 1, it can be found that the heat conductive polymer material prepared by the invention has good heat conductive property.
By comparison, examples 1, 2 and 3 have high thermal conductivity compared with comparative example 1, which illustrates that the nano aluminum oxide whisker and nylon 6 are modified, and are copolymerized and crosslinked to form a crosslinked network, so that the compatibility of the nano aluminum oxide whisker in nylon 6 is improved, the interface thermal resistance of the nylon 6 and the aluminum oxide nano whisker is reduced, and the thermal conductivity of the polymer material is improved.
Test example 2
Testing of mechanical Properties
The testing method comprises the following steps: the tensile strength of the composite material was tested according to the national standard GB/T1040-1992, and the tensile rate of the electronic universal tester was set to 50mm/min. The bending strength of the composite material is tested according to the national standard GB/T9341-2000, the bending speed is 2mm/min, and the positioning movement is set to be 6mm. The composite material was tested for notched impact strength according to national standard GB/T1043-1993, pendulum energy of 4.0J, and notch depth of 2mm. The results of the test are the average of 5 test results. The results are shown in Table 2.
TABLE 2
From the comparison of experimental data of examples 1 to 3 and comparative examples 1 to 3 in Table 2, it can be found that the heat conducting polymer material prepared by the invention has good mechanical properties.
By comparison, examples 1, 2 and 3 are better in tensile strength and bending strength compared with comparative example 1, and it is demonstrated that after modification of nano alumina whiskers and nylon 6 and polymerization between nano alumina whiskers and nylon 6 to generate a crosslinked network, on one hand, interfacial interaction between nano alumina whiskers and nylon 6 is enhanced, on the other hand, nano alumina whiskers tend to disperse, so that bending strength of a composite material is enhanced and bearing capacity before fracture is enhanced when bending stress is applied, while in comparative example 1, interaction between nano alumina whiskers and nylon 6 is weaker, internal defects are more, certain aggregation occurs after nano alumina whiskers are doped, rigidity of the composite material is increased, and tensile strength and bending strength are reduced; examples 1, 2, and 3 have better tensile strength and flexural strength than comparative example 2 because the nylon 6 and nano alumina whiskers do not form a cross-linked network, and the interface between them is weaker, and thus the tensile strength and flexural strength are lower.
By comparison, examples 1, 2 and 3 compared with comparative example 1 show that the nano-alumina whiskers and nylon 6 are modified, and after the nano-alumina whiskers and nylon 6 are polymerized to form a crosslinked network, the nylon 6 has good compatibility with the nano-alumina whiskers, and when a sample is impacted to generate cracks, the crosslinked network formed between the nylon 6 and the nano-alumina whiskers can absorb a large amount of energy, so that the nano-alumina whiskers cannot develop into destructive cracks, and the toughness of the composite material can be remarkably improved. While the nano alumina whiskers in comparative example 1, as a rigid filler, could not be deformed under stress, resulting in an increase in brittleness of the composite material, and thus in a decrease in impact strength. Examples 1, 2 and 3 have a higher impact strength than comparative example 2 because the nylon 6 and the nano alumina whiskers do not form a crosslinked network, and thus the impact strength of comparative example 2 is lower than examples 1 to 3.
Test example 3
Test of heat resistance
The testing method comprises the following steps: according to GB/T1634.1-2004, testing is carried out at a heating rate of 120 ℃/h and a load of 0.45MPa, and the average value of three sample bars is taken, wherein the difference between the three test data cannot exceed 5 ℃. The results are shown in Table 3.
TABLE 3 Table 3
| Sample of | HDT/℃ | Sample of | HDT/℃ |
| Example 1 | 252.6 | Comparative example 1 | 142.6 |
| Example 2 | 253.4 | Comparative example 2 | 176.2 |
| Example 3 | 252.8 | Comparative example 3 | 95.3 |
From the comparison of the experimental data of examples 1 to 3 and comparative examples 1 to 3 in Table 2, it can be found that the heat conductive polymer material prepared by the invention has good heat resistance.
By comparison, examples 1, 2 and 3 have higher heat distortion temperature than comparative example 1, because the modified nano alumina whisker has rigid structures such as maleimide and benzene ring on the grafted hyperbranched polyphosphazene network, and the crystallinity of nylon 6 can be improved, thereby leading to the improvement of heat distortion temperature; examples 1, 2 and 3 have higher heat distortion temperature than comparative example 2, and the examples modify nano alumina whiskers and nylon 6, and after the nano alumina whiskers and nylon 6 are polymerized to form a crosslinked network, the degree of freedom of nylon 6 molecular chains is limited, and movement of nylon 6 molecules is blocked, so that the heat distortion temperature is increased.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (10)
1. The heat conducting polymer material is characterized by being prepared by mixing modified nano aluminum oxide whisker, modified nylon 6 and potassium persulfate.
2. The heat conducting polymer material as claimed in claim 1, wherein the modified nano alumina whisker is prepared by pretreating nano alumina whisker with a silane coupling agent hydrolysis solution, reacting with p-phenylenediamine and phosphorus oxychloride, and reacting with maleic anhydride.
3. The heat conducting polymer material as claimed in claim 1, wherein the modified nylon 6 is prepared by grinding nylon 6 master batch into powder by a pulverizer, treating with formaldehyde alkaline mixed solution, reacting with trimethoxysilane, and reacting with vinyl silicone oil.
4. The heat conducting polymer material as claimed in claim 2, wherein the silane coupling agent hydrolysis solution is prepared by hydrolyzing aminopropyl triethoxysilane in 70-80% ethanol solution by mass fraction.
5. A thermally conductive polymer material as claimed in claim 3 wherein said aqueous formaldehyde base is prepared from sodium hydroxide and 10% aqueous formaldehyde by mass.
6. The preparation method of the heat conducting polymer material is characterized by comprising the following preparation steps:
(1) Mixing aminopropyl triethoxysilane and 70-80% ethanol according to a mass ratio of 5:150-180, and stirring at 45-55 ℃ for 30-40 min at 200-300 r/min to obtain a silane coupling agent hydrolysis solution; mixing nano alumina whisker and silane coupling agent hydrolysis solution according to a mass ratio of 1:40-50, stirring for 5-7 h at a temperature of 80-90 ℃ at a speed of 200-300 r/min, filtering, washing for 3-5 times by absolute ethyl alcohol, and drying for 3-5 h at a temperature of 80-90 ℃ to obtain pretreated nano alumina whisker; the pretreated nano alumina whisker, p-phenylenediamine, phosphorus oxychloride, triethylamine and chloroform are mixed according to the mass ratio
1:10-12:15-18:15-18:150-200, stirring at 200-300 r/min for 20-30 min at 0-5 ℃ to uniformly mix, stirring at 200-300 r/min for reacting for 5-7 h at 50-60 ℃, filtering, respectively washing for 3-5 times by pure water and absolute ethyl alcohol, and drying at 75-85 ℃ for 10-14 h to obtain the pre-modified nano alumina whisker; uniformly mixing maleic anhydride, N-dimethylformamide, pre-modified nano alumina whisker and toluene according to a mass ratio of 1:5-6:6-7:100-120, stirring and refluxing for 6-8 hours at a temperature of between 40 and 50 ℃ at a speed of between 200 and 300r/min, filtering, washing for 3 to 5 times by using absolute ethyl alcohol, and drying for 5 to 6 hours at a temperature of between 30 and 40 ℃ to obtain the modified nano alumina whisker;
(2) Grinding the nylon 6 master batch into powder with the particle size smaller than 100 mu m by a pulverizer, immersing the powder into formaldehyde alkaline mixed solution, stirring for 2-3 hours at 80-90 ℃ and 200-300 r/min, filtering, washing for 3-5 times by pure water, and drying for 5-6 hours at 50-60 ℃ to obtain pretreated nylon 6; stirring pretreated nylon 6, trimethoxysilane and absolute ethyl alcohol according to the mass ratio of 1:5-6:20-25 at 50-60 ℃ for reaction for 3-5 hours at 200-300 r/min, filtering, washing with absolute ethyl alcohol for 3-5 times, and drying at 50-60 ℃ for 5-6 hours to obtain the pre-modified nylon 6; mixing the pre-modified nylon 6, vinyl silicone oil and chloroplatinic acid according to the mass ratio of 1:12-13:0.001-0.002, stirring at the temperature of 100-120 ℃ for reaction for 6-8 hours at the speed of 200-300 r/min, filtering, washing with absolute ethyl alcohol for 3-5 times, and drying at the temperature of 50-60 ℃ for 5-6 hours to obtain modified nylon 6;
(3) Drying the modified nano alumina whisker and the modified nylon 6 at 75-85 ℃ for 10-12 hours respectively, uniformly mixing the modified nano alumina whisker, the modified nylon 6 and the potassium persulfate according to the mass ratio of 1-2:10-13:0.01-0.02, extruding and injecting the mixture into a polytetrafluoroethylene template at 250-300 r/min by a double screw extruder at 280-320 ℃, cooling to 80-90 ℃ and preserving heat for 20-24 hours, naturally cooling to room temperature, and demoulding and taking out to obtain the heat conducting polymer material.
7. The method for preparing a heat conducting polymer material according to claim 6, wherein the purity of the nano alumina whisker in the step (1) is more than 99.9%, and the nano alumina whisker is in a hexagonal crystal form.
8. The method for preparing a heat conducting polymer material according to claim 6, wherein the nylon 6 master batch in the step (2) is N477565; the model of the vinyl silicone oil is YDYH-VI421.
9. The method for preparing a heat conducting polymer material according to claim 6, wherein the method for preparing the silane coupling agent hydrolysis solution in step (1) comprises the following steps: mixing aminopropyl triethoxysilane and 70-80% ethanol according to a mass ratio of 5:150-180, and stirring at 45-55 ℃ for 30-40 min at 200-300 r/min.
10. The method for preparing a heat conducting polymer material according to claim 6, wherein the method for preparing the formaldehyde-alkaline mixed solution in the step (2) is as follows: the aqueous solution of sodium hydroxide and formaldehyde with the mass fraction of 10 percent is stirred for 30 to 40 minutes at the room temperature with the mass ratio of 200 to 300r/min according to the mass ratio of 1:45 to 55.
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