CN114395242A - High-thermal-conductivity POK composite material and preparation method and application thereof - Google Patents
High-thermal-conductivity POK composite material and preparation method and application thereof Download PDFInfo
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- CN114395242A CN114395242A CN202210144674.3A CN202210144674A CN114395242A CN 114395242 A CN114395242 A CN 114395242A CN 202210144674 A CN202210144674 A CN 202210144674A CN 114395242 A CN114395242 A CN 114395242A
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- 239000002131 composite material Substances 0.000 title claims abstract description 66
- 238000002360 preparation method Methods 0.000 title claims abstract description 35
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 110
- 229920005989 resin Polymers 0.000 claims abstract description 59
- 239000011347 resin Substances 0.000 claims abstract description 59
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 47
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 43
- 239000010439 graphite Substances 0.000 claims abstract description 43
- 239000002994 raw material Substances 0.000 claims abstract description 26
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 239000003365 glass fiber Substances 0.000 claims description 29
- 239000002245 particle Substances 0.000 claims description 16
- 239000003963 antioxidant agent Substances 0.000 claims description 15
- 230000003078 antioxidant effect Effects 0.000 claims description 15
- 238000001125 extrusion Methods 0.000 claims description 15
- 238000005469 granulation Methods 0.000 claims description 13
- 230000003179 granulation Effects 0.000 claims description 13
- 238000013329 compounding Methods 0.000 claims description 10
- 239000000314 lubricant Substances 0.000 claims description 9
- 239000000843 powder Substances 0.000 claims description 7
- 229910052799 carbon Inorganic materials 0.000 claims description 6
- 229910021382 natural graphite Inorganic materials 0.000 claims description 5
- OKOBUGCCXMIKDM-UHFFFAOYSA-N Irganox 1098 Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)NCCCCCCNC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 OKOBUGCCXMIKDM-UHFFFAOYSA-N 0.000 claims description 3
- 239000004594 Masterbatch (MB) Substances 0.000 claims description 3
- JKIJEFPNVSHHEI-UHFFFAOYSA-N Phenol, 2,4-bis(1,1-dimethylethyl)-, phosphite (3:1) Chemical compound CC(C)(C)C1=CC(C(C)(C)C)=CC=C1OP(OC=1C(=CC(=CC=1)C(C)(C)C)C(C)(C)C)OC1=CC=C(C(C)(C)C)C=C1C(C)(C)C JKIJEFPNVSHHEI-UHFFFAOYSA-N 0.000 claims description 3
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 claims description 3
- TXQVDVNAKHFQPP-UHFFFAOYSA-N [3-hydroxy-2,2-bis(hydroxymethyl)propyl] octadecanoate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(CO)(CO)CO TXQVDVNAKHFQPP-UHFFFAOYSA-N 0.000 claims description 3
- 229910021383 artificial graphite Inorganic materials 0.000 claims description 3
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 claims description 3
- 239000008116 calcium stearate Substances 0.000 claims description 3
- 235000013539 calcium stearate Nutrition 0.000 claims description 3
- 238000004891 communication Methods 0.000 claims description 3
- RKISUIUJZGSLEV-UHFFFAOYSA-N n-[2-(octadecanoylamino)ethyl]octadecanamide Chemical compound CCCCCCCCCCCCCCCCCC(=O)NCCNC(=O)CCCCCCCCCCCCCCCCC RKISUIUJZGSLEV-UHFFFAOYSA-N 0.000 claims description 3
- 229920001296 polysiloxane Polymers 0.000 claims description 3
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 claims description 3
- 239000000454 talc Substances 0.000 claims description 2
- 229910052623 talc Inorganic materials 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 33
- 239000000126 substance Substances 0.000 abstract description 16
- 238000010521 absorption reaction Methods 0.000 abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 9
- 230000007547 defect Effects 0.000 abstract description 3
- 238000001035 drying Methods 0.000 abstract description 3
- 229920000642 polymer Polymers 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 23
- 238000012545 processing Methods 0.000 description 14
- 239000004734 Polyphenylene sulfide Substances 0.000 description 10
- 229920000069 polyphenylene sulfide Polymers 0.000 description 10
- 239000006258 conductive agent Substances 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 5
- 239000004677 Nylon Substances 0.000 description 4
- 229920001778 nylon Polymers 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 239000003513 alkali Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000000155 melt Substances 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 239000002064 nanoplatelet Substances 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 230000017525 heat dissipation Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000011231 conductive filler Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 239000012815 thermoplastic material Substances 0.000 description 1
- 238000011282 treatment Methods 0.000 description 1
- 239000012856 weighed raw material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L73/00—Compositions of macromolecular compounds obtained by reactions forming a linkage containing oxygen or oxygen and carbon in the main chain, not provided for in groups C08L59/00 - C08L71/00; Compositions of derivatives of such polymers
-
- 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
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
-
- 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
Abstract
The invention relates to the technical field of modified polymer composite materials, and discloses a high-thermal-conductivity POK composite material and a preparation method thereof. The high-thermal-conductivity POK composite material comprises the following preparation raw materials: 40-64 parts of POK resin; 5-35 parts of graphene; 15-30 parts of graphite; 2.0-10.0 parts of a compatilizer. The preparation method of the high-thermal-conductivity POK composite material comprises the following steps: mixing the raw materials uniformly, extruding, granulating and drying. The composite material provided by the application has the advantages of good thermal conductivity, good chemical resistance, low water absorption, high toughness and the like, the defects of poor mechanical property, easiness in water absorption, poor size stability, high brittleness, poor chemical resistance and the like of the traditional heat conduction material are overcome, and the future application scene is wider.
Description
Technical Field
The invention relates to the technical field of modified polymer composite materials, in particular to a high-thermal-conductivity POK composite material and a preparation method and application thereof.
Background
POK resin (PK for short) is a novel polymer obtained by copolymerizing carbon monoxide, propylene and ethylene, due to the particularity of the molecular structure, the material has excellent chemical resistance, outstanding wear resistance, hydrolysis resistance and excellent low temperature resistance, and meets the requirements of low VOC and high barrier property, is a green environment-friendly material with more remote novel properties appearing in recent years, is used as a novel engineering plastic with outstanding wear resistance, the wear resistance of POK is 14 times that of POM, because of long-term dimensional stability, the POK can replace POM, nylon and other materials in the fields of pulleys, gears, bearings and the like, the performance retention rate of the POK material after water absorption is 30-40 percent higher than that of nylon, meanwhile, the C-C chain segment structure of the POK determines that the chemical properties of the POK are very stable, other chemical environments except strong acid and strong alkali can be basically tolerated, and the chemical resistance is basically equivalent to that of PPS. The melting point of the POK resin is about 220 ℃, so the POK resin can be used for a long time at 120 ℃, and the POK resin is widely applied to the fields of automobiles, electronics, electrics, communication and the like.
But with present scientific and technological development accelerate gradually, equipment is more and more high to the material heat dissipation requirement, traditional metal heat dissipation material weight is great, the cycle of processing is long, pollute greatly, now eliminated gradually, and POK is relatively poor as thermoplastic material's self heat conductivility, can't apply to in the reality, traditional heat conduction PA exists that the resistance to chemicals is poor, intensity and size receive the great shortcoming of environmental humidity influence, and the great problem of material fragility exists in the heat conduction PPS of commonly used, the use scene receives the restriction, consequently develop a new heat conduction plastics and be used for improving above problem thereby expand its application field and scene be the problem that present modified plastics field needs to solve urgently.
In view of this, the invention is particularly proposed.
Disclosure of Invention
The invention aims to provide a high-thermal-conductivity POK composite material and a preparation method and application thereof.
The invention is realized by the following steps:
in a first aspect, the present invention provides a high thermal conductivity POK composite material, which is prepared from the following raw materials:
in an alternative embodiment, the POK resin is prepared by compounding a high-viscosity resin and a low-viscosity resin in a ratio of 1: 1.5-2;
the high viscosity resin is POK resin with weight average molecular weight of 170000 and 190000; the low viscosity resin was a POK resin having a weight average molecular weight of 120000-140000.
In an optional embodiment, the graphene is in a micro-flake powder shape, and the number of the granular carbon layers is 10-20;
preferably, the thickness of the graphene particles is 5-100 nm, and the average particle size is 10-14 μm.
In an optional embodiment, the graphite takes the form of graphite powder as a raw material, and the average particle size of the graphite powder is 10-400 μm;
preferably, the graphite is one or two of natural graphite and synthetic graphite;
preferably, the carbon content of the graphite is greater than or equal to 95%.
In an alternative embodiment, the compatibilizing agent is at least one of POK-g-MAH, POE-g-MAH, and EMA-g-GMA.
In an alternative embodiment, preparing the feedstock further comprises: 0.1-0.3 part of antioxidant;
preferably, the antioxidant is at least one selected from the group consisting of antioxidant 1010, antioxidant 1098, antioxidant 168, antioxidant 9228, and antioxidant 2450.
In an alternative embodiment, preparing the feedstock further comprises: 0.3-2 parts of a lubricant;
preferably, the lubricant is selected from at least one of zinc stearate, calcium stearate, pentaerythritol stearate, ethylene bis stearamide, silicone master batch, and talc.
In an alternative embodiment, preparing the feedstock further comprises: 0.01-12 parts of glass fiber;
preferably, the glass fibers are selected from at least one of alkali-free continuous glass fibers and alkali-free chopped glass fibers;
preferably, the diameter of the alkali-free chopped glass fiber is 7-13 μm.
In a second aspect, the present invention provides a method for preparing a high thermal conductivity POK composite material according to the foregoing embodiment, including:
uniformly mixing the preparation raw materials, and extruding and granulating;
preferably, the preparation raw materials also comprise glass fibers, the extrusion granulation is twin-screw melt extrusion granulation, and the glass fibers are put into a twin-screw extruder from a side feeding cylinder;
preferably, the twin-screw extrusion temperature is set to 190-255 ℃, and the rotation speed of the main machine is 250-400 rpm.
In a third aspect, the present invention provides a high thermal conductivity POK composite material according to any one of the preceding embodiments or a high thermal conductivity POK composite material obtained by the preparation method according to the preceding embodiments, for use in the fields of automobiles, electronics, electricity, and communications.
The invention has the following beneficial effects:
the high-thermal-conductivity POK composite material mainly comprises POK resin, thermal-conductivity fillers graphene and graphite, and the thermal conductivity of the POK resin is improved by modifying the POK composite material through a thermal-conductivity agent; due to the fact that the graphene nanoplatelets are high in viscosity and poor in dispersibility, processing granulation is difficult and difficult due to the fact that graphene is added independently, meanwhile, the material is poor in flowing performance and processing performance, and the flowing performance and the processing performance of the material when the graphene and graphite are added into POK resin in a compounding mode are better than those when the graphene is added independently; after the graphene and the graphite with proper proportion are compounded, the heat conduction efficiency is higher than that of the compound with the graphite and the graphite which are independently added, the addition amount is smaller, and the formation of a heat conduction path is facilitated; the POK resin is mixed with graphite and graphene to have poor compatibility, the compatilizer in the components can improve the problem, the POK resin is treated by the compatilizer to have good compatibility with the graphene and the graphite, and the loss of mechanical properties is small. Therefore, the high-thermal-conductivity POK composite material has the advantages of good thermal conductivity, good chemical resistance, low water absorption, high toughness and the like. In addition, the C-C chain structure of the POK is more excellent in chemical resistance and acid and alkali resistance than those of heat-conducting nylon (PA) and heat-conducting polyphenylene sulfide (PPS), and can be used in a chemical solvent scene for a long time. Therefore, the composite material provided by the application overcomes the defects of poor mechanical property, easiness in water absorption, poor size stability, high brittleness, poor chemical resistance and the like of the traditional heat conducting material, and has a wider application scene in the future.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The high thermal conductivity POK composite material provided by the present application, and the preparation method and application thereof are specifically described below.
The high heat conduction POK composite material provided by the embodiment of the application comprises the following preparation raw materials:
the high-thermal-conductivity POK composite material mainly comprises POK resin, thermal-conductivity fillers graphene and graphite, and the thermal conductivity of the POK resin is improved by modifying the POK composite material through a thermal-conducting agent; due to the fact that the graphene nanoplatelets are high in viscosity and poor in dispersibility, processing granulation is difficult and difficult due to the fact that graphene is added independently, meanwhile, the material is poor in flowing performance and processing performance, and the flowing performance and the processing performance of the material when the graphene and graphite are added into POK resin in a compounding mode are better than those when the graphene is added independently; after the graphene and the graphite with proper proportion are compounded, the heat conduction efficiency is higher than that of the singly added graphite or the graphene, the addition amount is smaller, and the formation of a heat conduction path is facilitated; the POK resin is mixed with graphite and graphene to have poor compatibility, the compatilizer in the components can improve the problem, the POK resin is treated by the compatilizer to have good compatibility with the graphene and the graphite, and the loss of mechanical properties is small. In conclusion, the high-thermal-conductivity POK composite material provided by the application has the advantages of good thermal conductivity, excellent chemical resistance, low water absorption, high toughness and the like. Compared with traditional heat conduction materials such as PA, PPS and PP, the composite material has better comprehensive performance.
Preferably, the POK resin is prepared by compounding a high-viscosity resin and a low-viscosity resin in a ratio of 1: 1.5-2 (such as 1:1.5, 1:1.7 or 1: 2);
the high viscosity resin is a POK resin having a weight average molecular weight of 170000 and 190000 (e.g., 170000, 180000, or 190000); the low viscosity resin is a POK resin having a weight average molecular weight of 120000-140000 (e.g., 120000, 130000, or 140000).
The high-viscosity resin has the notch impact strength kept at 11-13 KJ/m under the condition of 240 ℃/2.16kg melt index test of 60-70 g/10min2(ii) a The low viscosity resin is described inThe notched impact strength is kept between 5 and 7KJ/m at 180 to 200g/10min under the condition of 240 ℃/2.16kg melt index test2。
The resin with higher weight average molecular weight has high viscosity, and the POK composite material with high heat conductivity, good processing fluidity, good impact resistance and high molding precision can be obtained by compounding the POK resins with different weight average molecular weight viscosities in a proper proportion in the preferred embodiment of the application.
Preferably, in order to obtain the high thermal conductivity POK composite material with better thermal conductivity and physical properties, the graphene is in a form of microchip powder, and the number of the granular carbon layers is 10-20 (for example, 10, 15 or 20). Further, the graphene has a particle thickness of 5 to 100nm (e.g., 5nm, 10nm, 50nm, or 100nm) and an average particle diameter of 10 to 14 μm (e.g., 10 μm, 12 μm, or 14 μm).
In order to obtain a high thermal conductivity POK composite material with better thermal conductivity and physical properties, graphite is used as a raw material, generally, the larger the particle size of graphite powder is, the easier it is to form a thermal conduction channel in the material and further the higher the thermal conductivity is, but the lower the mechanical properties of the material are, so a suitable particle size range needs to be determined when selecting graphite powder, in a preferred embodiment of the present application, the average particle size of graphite powder is 10 to 400 μm (e.g., 10 μm, 50 μm, 100 μm, or 400 μm); specifically, the graphite is one or two of natural graphite and synthetic graphite; further, the carbon content of the graphite is greater than or equal to 95%.
Preferably, in order to ensure better compatibility of the POK resin, the graphene and the graphite, the compatilizer is at least one of POK-g-MAH, POE-g-MAH and EMA-g-GMA.
Further, in order to improve the oxidation resistance of the composite material, the preparation raw materials further comprise: 0.1-0.3 part of antioxidant. Specifically, the antioxidant is at least one selected from the group consisting of antioxidant 1010, antioxidant 1098, antioxidant 168, antioxidant 9228 and antioxidant 2450.
Furthermore, in order to improve the lubrication degree of each component in the high-thermal-conductivity POK composite material, the influence of graphene and graphite on the viscosity of the melt is reduced, and the melt extrusion is facilitated. The preparation raw materials also comprise: 0.3-2 parts of a lubricant. Specifically, the lubricant is at least one selected from zinc stearate, calcium stearate, pentaerythritol stearate, ethylene bis-stearamide, silicone master batch and talc powder.
Further, in order to improve the mechanical properties of the composite material, the preparation raw materials further comprise: 0.01-12 parts of glass fiber. Preferably, the glass fibers are selected from at least one of alkali-free continuous glass fibers and alkali-free chopped glass fibers; when the glass fiber is alkali-free chopped glass fiber, the diameter of the alkali-free chopped glass fiber is 7-13 mu m.
The preparation method of the high-thermal-conductivity POK composite material provided by the embodiment of the application comprises the following steps:
the preparation raw materials are uniformly mixed and extruded for granulation.
The preparation method specifically comprises the following steps:
s1, weighing the corresponding POK resin, graphene, graphite, a compatilizer, an antioxidant, a lubricant and glass fiber according to the weight parts of the components described in the content, wherein the ratio of the high-viscosity resin to the low-viscosity resin is 1: 1.5-2.
S2, mixing the weighed POK resin, graphene, graphite, a compatilizer, an antioxidant and a lubricant to obtain a mixed material.
And S3, adding the glass fiber into the mixed material from the side feeding port, and then extruding, melting, granulating, drying and processing by a double screw to obtain the high-thermal-conductivity POK composite material.
Preferably, the extrusion equipment for mixing the materials is a twin screw extruder. In the case of extrusion granulation in a twin-screw extruder, the glass fiber may be fed from a side feed port, or if the glass fiber is continuous, the glass fiber may be fed from an exhaust port.
Further, the rotation speed of the main machine is set to be 250-400rpm (for example, 250rpm, 300rpm or 400rpm) in the extrusion granulation process, and the twin-screw extrusion temperature is set to be 190-255 ℃ (for example, 190 ℃, 200 ℃, 230 ℃ or 255 ℃).
Further, in order to obtain a good granulation effect, the twin-screw extrusion temperature is set from the feeding section to the machine head as follows in sequence: 210 deg.C, 245 deg.C, 240 deg.C, 235 deg.C, 250 deg.C.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
The high-thermal-conductivity POK composite material comprises the following preparation raw materials in parts by weight:
wherein, POK resin (low viscosity) is POK resin with weight average molecular weight of 130000, and POK resin (high viscosity) is POK resin with weight average molecular weight of 180000; the average particle size of the graphene powder was 14 μm, and the average particle size of the graphite was 10 μm.
The preparation method comprises the following steps:
weighing the POK resin, the graphene, the graphite, the compatilizer, the antioxidant, the lubricant and the glass fiber according to the proportion.
And (3) mixing the weighed raw materials except the glass fiber to obtain a mixed material.
Glass fiber is put into the mixed material from a side feeding port, and the rotating speed of a main machine is set to be 250 rpm. The twin-screw extrusion temperature is set from the feeding section to the machine head as follows: 210 ℃, 245 ℃, 240 ℃, 235 ℃, 250 ℃, and then carrying out twin-screw extrusion, melting, granulation, drying and treatment to obtain the high-thermal-conductivity POK composite material.
Example 2
The high-thermal-conductivity POK composite material comprises the following preparation raw materials in parts by weight:
nothing in this example is the same as example 1.
Example 3
The high-thermal-conductivity POK composite material comprises the following preparation raw materials in parts by weight:
nothing in this example is the same as example 1.
Example 4
The high-thermal-conductivity POK composite material comprises the following preparation raw materials in parts by weight:
nothing in this example is the same as example 1.
Example 5
The high-thermal-conductivity POK composite material comprises the following preparation raw materials in parts by weight:
in this example, the average particle size of the natural graphite powder was 400 μm.
Nothing in this example is the same as example 1.
Example 6
The high-thermal-conductivity POK composite material comprises the following preparation raw materials in parts by weight:
in this example, the average particle size of the natural graphite powder was 400 μm.
Nothing in this example is the same as example 1.
Example 7
The high-thermal-conductivity POK composite material comprises the following preparation raw materials in parts by weight:
nothing in this example is the same as example 1.
Comparative example 1
This comparative example is essentially the same as example 6, except that: no compatibilizer was added.
Comparative example 2
This comparative example is substantially the same as comparative example 1 except that: the graphite powder and the graphene powder are completely replaced by 50 parts of graphite powder, and the graphite powder does not contain a compatilizer.
Comparative example 3
This comparative example is substantially the same as the example except that the graphene powder was completely replaced with graphite powder in an equal amount.
Comparative example 4
This comparative example is substantially the same as the example except that the graphite powder was completely replaced with the same amount of graphene powder.
Comparative example 5
This comparative example is essentially the same as the examples, except that: the preparation raw materials do not comprise graphite, graphene and a compatilizer.
Examples of the experiments
The method is carried out by a double-screw extrusion granulation injection molding method according to ISO standard. The properties of the POK resins obtained in examples 1 to 7 and comparative examples 1 to 3 were tested, and the results are reported in tables 1 to 2.
TABLE 1 Properties of the composites obtained in the examples
TABLE 2 Properties of the composites prepared in each comparative example
TABLE 3 results of performance test (85% RH, 24h) of composites prepared in examples and comparative examples after water absorption
The heat conductivity coefficient of the existing PPS material is about 3.0w, and the tensile strength is about 30 MPa; the heat conductivity coefficient of the existing PA material is about 3.0w, and the tensile strength is about 38 MPa. As can be seen from the table above, the composite material prepared in the embodiments 1 to 7 has high mechanical property and thermal conductivity, the mechanical property of the composite material is superior to that of the existing PPS material and PA material, and the thermal conductivity of the composite material is equivalent to that of the existing PPS material and PA material.
Comparing the example 6 with the comparative example 1, it can be seen that the thermal conductivity of the prepared composite material is obviously poor without adding the compatilizer, which indicates that the compatibility of the material with graphene and graphite is improved after the material is treated by the compatilizer, and the loss of mechanical properties is small; as can be seen by comparing several examples, the change of the ratio of the low viscosity and the high viscosity of the POK resin has obvious influence on the melt index of the composite material, so that the ratio relationship of the low viscosity and the high viscosity resin can be adjusted according to the specific melt index requirement during production to obtain the composite material with good processing flowability and impact resistance and high molding precision. Comparing comparative example 1 with comparative example 2, it can be seen that, even if the addition amount is larger when the heat conducting agent is only graphite, the heat conducting effect is poorer when the heat conducting agent is graphite and graphene compounded. Comparing the example 1 with the comparative example 3, it can be seen that the mechanical property of the composite material of the comparative example 3 is worse, which shows that the property of the material prepared by compounding the conductive agent graphene and graphite is better than that of the material prepared by compounding the conductive agent graphene only; comparing example 1 with comparative example 4, it can be seen that the composite material of comparative example 4 has poorer flow and processing properties, which indicates that the material prepared by compounding graphene and graphite as the conductive agent has better performance than graphite as the conductive agent. Comparing example 1 with comparative example 5, the thermal conductivity of comparative example 5 is worse, and the specification adopts the conductive agent to modify the POK resin, so that better comprehensive mechanical property and thermal conductivity can be obtained.
In summary, the high thermal conductivity POK composite material provided by the embodiment of the application mainly comprises POK resin, thermal conductive fillers graphene and graphite, and the thermal conductivity of the POK resin is improved by modifying the POK composite material through the thermal conductive agent; due to the fact that the graphene nanoplatelets are high in viscosity and poor in dispersibility, processing granulation is difficult and difficult due to the fact that graphene is added independently, meanwhile, the material is poor in flowing performance and processing performance, and the flowing performance and the processing performance of the material when the graphene and graphite are added into POK resin in a compounding mode are better than those when the graphene is added independently; after the graphene and the graphite with proper proportion are compounded, the heat conduction efficiency is higher than that of the compound with the graphite and the graphite which are independently added, the addition amount is smaller, and the formation of a heat conduction path is facilitated; the POK resin is mixed with graphite and graphene to have poor compatibility, the compatilizer in the components can improve the problem, the POK resin is treated by the compatilizer to have good compatibility with the graphene and the graphite, and the loss of mechanical properties is small. Therefore, the high-thermal-conductivity POK composite material has the advantages of good thermal conductivity, good chemical resistance, low water absorption, high toughness and the like. In addition, the C-C chain structure of the POK is more excellent in chemical resistance and acid and alkali resistance than those of heat-conducting nylon (PA) and heat-conducting polyphenylene sulfide (PPS), and can be used in a chemical solvent scene for a long time. Therefore, the composite material provided by the application overcomes the defects of poor mechanical property, easiness in water absorption, poor size stability, high brittleness and poor chemical resistance of the traditional heat conducting material, and has a wider application scene in the future.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The high-thermal-conductivity POK composite material is characterized by comprising the following preparation raw materials:
2. the POK composite material with high thermal conductivity as claimed in claim 1, wherein the POK resin is prepared by compounding high-viscosity resin and low-viscosity resin in a ratio of 1: 1.5-2;
the high-viscosity resin is POK resin with the weight-average molecular weight of 170000 and 190000; the low-viscosity resin is a POK resin with a weight-average molecular weight of 120000-140000.
3. The POK composite material with high thermal conductivity as claimed in claim 1, wherein the graphene is in a form of micro-flake powder, and the number of carbon particles is 10-20;
preferably, the particle thickness of the graphene is 5-100 nm, and the average particle size is 10-14 μm.
4. The POK composite material with high thermal conductivity as claimed in claim 1, wherein the graphite is in the form of graphite powder, and the average particle size of the graphite powder is 10-400 μm;
preferably, the graphite is one or two of natural graphite and synthetic graphite;
preferably, the graphite contains carbon in an amount greater than or equal to 95%.
5. The POK composite material of claim 1, wherein the compatibilizer is at least one of POK-g-MAH, POE-g-MAH, and EMA-g-GMA.
6. The high thermal conductivity POK composite material as claimed in claim 1, wherein the raw materials for preparation further comprise: 0.1-0.3 part of antioxidant;
preferably, the antioxidant is at least one selected from the group consisting of antioxidant 1010, antioxidant 1098, antioxidant 168, antioxidant 9228, and antioxidant 2450.
7. The high thermal conductivity POK composite material as claimed in claim 1, wherein the raw materials for preparation further comprise: 0.3-2 parts of a lubricant;
preferably, the lubricant is selected from at least one of zinc stearate, calcium stearate, pentaerythritol stearate, ethylene bis stearamide, silicone master batch, and talc.
8. The high thermal conductivity POK composite material as claimed in claim 1, wherein the raw materials for preparation further comprise: 0.01-12 parts of glass fiber;
preferably, the glass fibers are selected from at least one of alkali-free continuous glass fibers and alkali-free chopped glass fibers;
preferably, the diameter of the alkali-free chopped glass fiber is 7-13 μm.
9. The preparation method of the high thermal conductivity POK composite material as claimed in any one of claims 1 to 7, comprising the following steps:
uniformly mixing the preparation raw materials, and extruding and granulating;
preferably, the preparation raw materials further comprise glass fibers, the extrusion granulation is twin-screw melt extrusion granulation, and the glass fibers are fed into a twin-screw extruder from a side feeding barrel;
preferably, the twin-screw extrusion temperature is set to 190-255 ℃, and the rotation speed of the main machine is 250-400 rpm.
10. The high thermal conductivity POK composite material as claimed in any one of claims 1 to 8 or the high thermal conductivity POK composite material prepared by the preparation method as claimed in claim 9 is applied to the fields of automobiles, electronics, electrics and communications.
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| CN115260734A (en) * | 2022-09-27 | 2022-11-01 | 广东盟信塑胶实业有限公司 | Wear-resistant anti-deformation POK plastic bar and preparation method thereof |
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| CN107915973A (en) * | 2016-10-08 | 2018-04-17 | 中国石油化工股份有限公司 | Thermoplasticity heat-conductive resin composition and preparation method thereof |
| CN109851985A (en) * | 2018-11-28 | 2019-06-07 | 金旸（厦门）新材料科技有限公司 | A kind of fire-retardant thermally conductive polyketone composite material and preparation method of enhancing |
| WO2021107894A1 (en) * | 2019-11-27 | 2021-06-03 | İzmi̇r Eği̇ti̇m Sağlik Sanayi̇ Yatirim A.Ş. | Polymer-based composite material with high thermal conductivity |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107915973A (en) * | 2016-10-08 | 2018-04-17 | 中国石油化工股份有限公司 | Thermoplasticity heat-conductive resin composition and preparation method thereof |
| CN109851985A (en) * | 2018-11-28 | 2019-06-07 | 金旸（厦门）新材料科技有限公司 | A kind of fire-retardant thermally conductive polyketone composite material and preparation method of enhancing |
| WO2021107894A1 (en) * | 2019-11-27 | 2021-06-03 | İzmi̇r Eği̇ti̇m Sağlik Sanayi̇ Yatirim A.Ş. | Polymer-based composite material with high thermal conductivity |
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| CN115260734A (en) * | 2022-09-27 | 2022-11-01 | 广东盟信塑胶实业有限公司 | Wear-resistant anti-deformation POK plastic bar and preparation method thereof |
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