CN102558609B - Method for improving thermal conductivity of thermal conductive polymer - Google Patents
Method for improving thermal conductivity of thermal conductive polymer Download PDFInfo
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- CN102558609B CN102558609B CN 201110414293 CN201110414293A CN102558609B CN 102558609 B CN102558609 B CN 102558609B CN 201110414293 CN201110414293 CN 201110414293 CN 201110414293 A CN201110414293 A CN 201110414293A CN 102558609 B CN102558609 B CN 102558609B
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Abstract
The invention discloses a method for improving thermal conductivity of thermal conductive polymer. The method comprises the following steps of: adding a polymer substrate into a high speed mixer, adding a thermal conductive filler and other additives into the high speed mixer, continuously mixing uniformly, and feeding into a main feeding port of a double-screw extruder; controlling the ratio of a reinforcing component to the nanometer thermal conductive filler to be 20:1-5:1, adding the reinforcing component into the high speed mixer, adding the nanometer thermal conductive filler and a surface modifier, continuously mixing to ensure that the thermal conductive filler is adhered to the surface of the reinforcing component, uniformly mixing, and feeding into a side feeding port of the double-screw extruder; and performing melt blending on raw material components by using the double-screw extruder, extruding, performing water cooling, pelletizing, sieving, packaging and the like to obtain the thermal conductive polymer with improved thermal conductivity. The thermal conductive polymer prepared by the method has the improved thermal conductivity and keeps high mechanical properties.
Description
Technical field
The present invention relates to a kind of preparation method who improves the thermal conductive polymer heat conductivility, belong to the functional high molecule material technical field.
Background technology
In recent years, utilize the heat conduction component that polymeric matrix is filled the polymer composites that has a high thermal conductivity with preparation and obtained more and more widely concern.In order to prepare the polymer materials of high thermal conductivity, a lot of researchs and invention often take to improve the preparation method of heat conduction component loading level, to reach the purpose that improves heat conductivility.Patent CN1775860A discloses a kind of " moulded heat-conductive insulated plastics of injection moulding ", and this invention is added MgO, Al in thermoplasticss such as PPS, PA, PBT, ABS or PP
2O
3Deng heat conductive filler commonly used, wherein the mass parts of plastic substrate is 100, and the mass parts of heat conductive filler is 100-700, and heat conductive filler shared massfraction in thermally conductive material is 50-87.5%; Patent CN101280109A discloses a kind of " electrostatic-resistant heat conducting plastic ", the method of this patent disclosure is: add the low zinc sulphide of hardness and obtain the PPS heat-conducting plastic in the PPS resin, when the content of heat conductive filler is up to 75wt% in the invention, thermal conductivity is less than 1.0W/m.K, with respect to the amplitude that improves addition, thermal conductivity improves less.In addition, add the mechanical properties decrease that high-load heat conductive filler tends to make material.Patent CN101280108A discloses a kind of heat-conducting plastic with high mechanical strength, this invention is under the situation of adding high-content heat conductive filler MgO, add roving glass fiber simultaneously and improve the physical strength of material, but this invention does not mention how preparing to have the more heat-conducting plastic of high thermal conductivity coefficient in this system.
The present invention prepares thermal conductive polymer by specific preparation method on the prior art basis, than other preparation methods, its thermal conductive polymer of preparing not only has high characteristics of filling high-mechanical property, and has improved heat conductivility.
Summary of the invention
The purpose of this invention is to provide a kind of preparation method who improves the thermal conductive polymer heat conductivility, the thermal conductive polymer of this method preparation has good mechanical performance and improved heat conductivility.
To achieve these goals, the present invention adopts following technical scheme:
A kind of method that improves the thermal conductive polymer heat conductivility may further comprise the steps:
(1) prepare material, take by weighing each material by following weight percentage:
Polymeric matrix 20-45%
Heat conductive filler 30-70%
Nano heat-conductive filler 0.25-5%
Enhancement component 5-20%
Surface-modifying agent 0.1-0.5%
Other additives 1-15 %
Wherein the part by weight of enhancement component and nano heat-conductive filler is controlled in the 20:1-5:1 scope; Above-mentioned each component percentage composition meter summation by weight is 100%;
(2) polymeric matrix is joined in the high-speed mixer,, continue to mix the main spout that the back is expected twin screw extruder down then to wherein adding heat conductive filler and other additives;
(3) enhancement component is joined in the high-speed mixer, continue to mix to wherein adding nano heat-conductive filler and surface-modifying agent then, make heat conductive filler adhere to the surface of enhancement component, expect the side spout of twin screw extruder then down;
(4) each component starting material is extruded behind the twin screw extruder melt blending, passes through water-cooled, pelletizing, sieves, adorns bag, the preparation thermal conductive polymer.
In aforesaid method, described polymeric matrix is one or more the mixture in polyphenylene sulfide (PPS), liquid crystalline polymers (LCP), polymeric amide (as PA10T, PA6T/66, PA6T/6I, PA9T, PA46, PA6, PA66, PA6/66, PA12, PA6/12), polyester (as PBT, PET, PC), styrenic polymer (as ABS, PS) and the polyolefine (as PP, PE), but is not limited only to these plastic substrates;
In aforesaid method, the median size of described heat conductive filler is 1-50 μ m, comprises aluminium powder, copper powder, iron powder, graphite, aluminum oxide (Al
2O
3), magnesium oxide (MgO), zinc oxide (ZnO), aluminium nitride (AlN), boron nitride (BN), silicon carbide (SiC), zinc sulphide (ZnS), magnesium hydroxide (Mg(OH)
2), aluminium hydroxide (Al(OH)
3), Calcium Fluoride (Fluorspan) (CaF
2) in waiting one or more, but be not limited only to these heat conductive fillers;
In aforesaid method, the median size of described nano heat-conductive filler is 30-80nm, comprises aluminum oxide (Al
2O
3), a kind of in the magnesium oxide (MgO), zinc oxide (ZnO), aluminium nitride (AlN), boron nitride nano heat-conductive fillers such as (BN), but be not limited only to these nano heat-conductive fillers;
In aforesaid method, described surface-modifying agent is one or more mixing in aromatic sulphonate, aromatic sulfonamide, silane coupling agent, aluminate coupling agent, the titanate coupling agent, but is not limited only to these surface-modifying agents;
In aforesaid method, described other additives comprise one or more mixing in fire retardant, fire retarding synergist, lubricant, the oxidation inhibitor.Described fire retardant comprises a kind of in brominated Polystyrene, brominated polystyrene and brominated polyphenylene ether resin, the phosphinates; Described fire retarding synergist comprises one or more in ANTIMONY TRIOXIDE SB 203 99.8 PCT, zinc borate, zinc, zinc oxide, sodium antimonate, boehmite, the tetrafluoroethylene; Described lubricant comprises one or more in lignite acid derivative, macromolecule wax class, low molecular weight liquid crystal polymkeric substance, metallic soap of stearic acid salt, stearic amide, the silicone compound; Described oxidation inhibitor comprises one or more in Hinered phenols antioxidant, suffocated amine antioxidant, phosphite ester kind antioxidant, thiodipropionate antioxidant or the thio-alcohol oxidation inhibitor.
In aforesaid method, described enhancement component is one or more in short glass fiber, carbon fiber, wollastonite fibre, lime carbonate, talcum powder, silicon-dioxide, mica, the potassium titanate crystal whisker etc., but is not limited only to these reinforcing fillers.
Compared with prior art, the present invention has following advantage:
The nano heat-conductive filler that the present invention utilizes the surface-modifying agent handle to have high thermal conductivity adheres to the enhancement component surface of low thermal conductivity, forms the heat conduction enhancement component, thereby improves its capacity of heat transmission.When enhancement component is scattered in the polymeric matrix, can play enhancement, can play the reinforcement heat transfer effect again, help improving the heat conductivility of thermal conductive polymer.Further, enhancement component is by its surperficial nano heat-conductive filler and the interaction that is dispersed in the heat conductive filler in the polymeric matrix, in the melt blending process, the heat conductive filler that is dispersed in the matrix is linked together, help isolated heat conduction particle is connected into the heat conduction network, make easier formation conducting network between filler component, improve the heat conductivility of material widely.
Embodiment
The invention will be further described below in conjunction with embodiment.
Embodiment 1
At first, take by weighing each material: polyphenylene sulfide 23.2wt%, magnesium oxide 65wt%, nano aluminium oxide 0.5wt%, short glass fiber 10wt%, silane coupling agent 0.3wt%, montanic acid wax 0.5wt%, oxidation inhibitor 0.5wt% by following weight percentage.
Then polyphenylene sulfide is added in the high-speed mixer,, continues to mix the main spout that the back is expected twin screw extruder down to wherein adding magnesium oxide, montanic acid wax and oxidation inhibitor; Equally glass fibre is joined in the high-speed mixer,, continue to mix the side spout that the back is expected twin screw extruder down to wherein adding nano aluminium oxide and silane coupling agent; Each component starting material prepares thermal conductive polymer through twin screw extruder melt blending extruding pelletization.
Every test result of the prepared thermal conductive polymer that gets of this embodiment sees Table 1.
Embodiment 2
At first, take by weighing each material: polyphenylene sulfide 22.7wt%, magnesium oxide 65wt%, nano aluminium oxide 1wt%, short glass fiber 10wt%, silane coupling agent 0.3wt%, montanic acid wax 0.5wt%, oxidation inhibitor 0.5wt% by following weight percentage.
Prepare thermal conductive polymer by embodiment 1 described preparation method then.
Every test result of the prepared thermal conductive polymer that gets of this embodiment sees Table 1.
Embodiment 3
At first, take by weighing each material: polyphenylene sulfide 21.7wt%, magnesium oxide 65wt%, nano aluminium oxide 2wt%, short glass fiber 10wt%, silane coupling agent 0.3wt%, montanic acid wax 0.5wt%, oxidation inhibitor 0.5wt% by following weight percentage.
Prepare thermal conductive polymer by embodiment 1 described preparation method then.
Every test result of the prepared thermal conductive polymer that gets of this embodiment sees Table 1.
Comparative Examples 1
At first, take by weighing each material: polyphenylene sulfide 23.7wt%, magnesium oxide 65wt%, short glass fiber 10wt%, silane coupling agent 0.3wt%, montanic acid wax 0.5wt%, oxidation inhibitor 0.5wt% by following weight percentage.
Then polyphenylene sulfide is added in the high-speed mixer,, continues to mix the main spout that the back is expected twin screw extruder down to wherein adding magnesium oxide, montanic acid wax and oxidation inhibitor; Equally glass fibre is joined in the high-speed mixer,, continue to mix the side spout that the back is expected twin screw extruder down to wherein adding silane coupling agent; Each component starting material prepares thermal conductive polymer through twin screw extruder melt blending extruding pelletization.
Every test result of the prepared thermal conductive polymer that gets of this Comparative Examples sees Table 1.
Comparative Examples 2
At first, take by weighing each material: polyphenylene sulfide 23wt%, magnesium oxide 65wt%, nano aluminium oxide 1wt%, short glass fiber 10wt%, montanic acid wax 0.5wt%, oxidation inhibitor 0.5wt% by following weight percentage.
Then polyphenylene sulfide is added in the high-speed mixer,, continues to mix the main spout that the back is expected twin screw extruder down to wherein adding magnesium oxide, montanic acid wax and oxidation inhibitor; Equally glass fibre is joined in the high-speed mixer,, continue to mix the side spout that the back is expected twin screw extruder down to wherein adding nano aluminium oxide; Each component starting material prepares thermal conductive polymer through twin screw extruder melt blending extruding pelletization.
Every test result of the prepared thermal conductive polymer that gets of this Comparative Examples sees Table 1.
Embodiment 4
At first, take by weighing each material: polyphenylene sulfide 31.7wt%, magnesium oxide 55wt%, nano aluminium oxide 2wt%, short glass fiber 10wt%, silane coupling agent 0.3wt%, montanic acid wax 0.5wt%, oxidation inhibitor 0.5wt% by following weight percentage.
Prepare thermal conductive polymer by embodiment 1 described preparation method then.
Every test result of the prepared thermal conductive polymer that gets of this embodiment sees Table 1.
Comparative Examples 3
At first, take by weighing each material: polyphenylene sulfide 33.5wt%, magnesium oxide 55wt%, nano aluminium oxide 0.2wt%, short glass fiber 10wt%, silane coupling agent 0.3wt%, montanic acid wax 0.5wt%, oxidation inhibitor 0.5wt% by following weight percentage.
Prepare thermal conductive polymer by embodiment 1 described preparation method then.
Every test result of the prepared thermal conductive polymer that gets of this embodiment sees Table 1.
Comparative Examples 4
At first, take by weighing each material: polyphenylene sulfide 30.2wt%, magnesium oxide 55wt%, nano aluminium oxide 3.5wt%, short glass fiber 10wt%, silane coupling agent 0.3wt%, montanic acid wax 0.5wt%, oxidation inhibitor 0.5wt% by following weight percentage.
Prepare thermal conductive polymer by embodiment 1 described preparation method then.
Every test result of the prepared thermal conductive polymer that gets of this embodiment sees Table 1.
Embodiment 5
At first, take by weighing each material: polymeric amide PA10T 42.5wt%, boron nitride 30wt%, nano aluminum nitride 2wt% by following weight percentage, wollastonite fibre 15wt%, aromatic sulfonamide 0.5wt%, diethyl phospho acid aluminium 8wt%, zinc 1wt%, silicone master batch 0.5wt%, oxidation inhibitor 0.5wt%.
Prepare thermal conductive polymer by embodiment 1 described preparation method then.
Every test result of the prepared thermal conductive polymer that gets of this embodiment sees Table 1.
Comparative Examples 5
At first, take by weighing each material: polymeric amide PA10T 44.5wt%, boron nitride 30wt% by following weight percentage, wollastonite fibre 15wt%, aromatic sulfonamide 0.5wt%, diethyl phospho acid aluminium 8wt%, zinc 1wt%, silicone master batch 0.5wt%, oxidation inhibitor 0.5wt%.
Prepare thermal conductive polymer by Comparative Examples 1 described preparation method then.
Every test result of the prepared thermal conductive polymer that gets of this embodiment sees Table 1.
Comparative Examples 6
At first, take by weighing each material: polymeric amide PA10T 43wt%, boron nitride 30wt%, nano aluminum nitride 2wt%, wollastonite fibre 15wt%, diethyl phospho acid aluminium 8wt%, zinc 1wt%, silicone master batch 0.5wt%, oxidation inhibitor 0.5wt% by following weight percentage.
Prepare thermal conductive polymer by Comparative Examples 2 described preparation methods then.
Every test result of the prepared thermal conductive polymer that gets of this embodiment sees Table 1.
Mechanical property adopts the omnipotent experiment test machine test of INSTRON, steps on stone trade Co., Ltd available from Shanghai;
The thermal conductivity test adopts Hot-disk TPS1500 type conductometer to measure.
Each embodiment of table 1 and Comparative Examples parameter testing result
Result from table as can be seen, than other preparation methods, the thermal conductive polymer by preparation method of the present invention preparation not only has improved heat conductivility, and has kept the good mechanical performance; Suitably with the ratio control of enhancement component and nano heat-conductive filler in the 20:1-5:1 scope, can obtain the effect of more excellent improvement thermal conductive polymer heat conductivility.
Claims (9)
1. method that improves the thermal conductive polymer heat conductivility is characterized in that may further comprise the steps:
(1) prepare material, take by weighing each material by following weight percentage:
Polymeric matrix 20-45%
Heat conductive filler 30-70%
Nano heat-conductive filler 0.25-5%
Enhancement component 5-20%
Surface-modifying agent 0.1-0.5%
Other additives 1-15 %
Wherein the part by weight of enhancement component and nano heat-conductive filler is controlled in the 20:1-5:1 scope; Above-mentioned each component percentage composition meter summation by weight is 100%;
(2) polymeric matrix is joined in the high-speed mixer,, continue to mix the main spout that the back is expected twin screw extruder down then to wherein adding heat conductive filler and other additives;
(3) enhancement component is joined in the high-speed mixer, continue to mix to wherein adding nano heat-conductive filler and surface-modifying agent then, make heat conductive filler adhere to the surface of enhancement component, expect the side spout of twin screw extruder then down;
(4) each component starting material is extruded behind the twin screw extruder melt blending, passes through water-cooled, pelletizing, sieves, adorns bag, the preparation thermal conductive polymer.
2. method according to claim 1 is characterized in that described polymeric matrix is one or more the mixture in polyphenylene sulfide, liquid crystalline polymers, polymeric amide, polyester and the polyolefine.
3. method according to claim 2 is characterized in that described polyolefine is a styrenic polymer.
4. method according to claim 1, it is characterized in that described heat conductive filler median size is 1-50 μ m, comprises one or more mixing in aluminium powder, copper powder, iron powder, graphite, aluminum oxide, magnesium oxide, zinc oxide, aluminium nitride, boron nitride, silicon carbide, zinc sulphide, magnesium hydroxide, aluminium hydroxide, the Calcium Fluoride (Fluorspan).
5. method according to claim 1 is characterized in that described nano heat-conductive filler median size is 30-80nm, comprises one or more mixing in aluminum oxide, magnesium oxide, zinc oxide, aluminium nitride, the boron nitride.
6. method according to claim 1 is characterized in that described enhancement component is one or more mixing in short glass fiber, carbon fiber, wollastonite fibre, lime carbonate, talcum powder, silicon-dioxide, mica, the potassium titanate crystal whisker.
7. method according to claim 1 is characterized in that described surface-modifying agent is one or more mixing in aromatic sulphonate, aromatic sulfonamide, silane coupling agent, aluminate coupling agent, the titanate coupling agent.
8. method according to claim 1 is characterized in that described other additives comprise one or more mixing in fire retardant, fire retarding synergist, lubricant, the oxidation inhibitor.
9. method according to claim 8 is characterized in that, described fire retardant comprises a kind of in brominated Polystyrene, brominated polystyrene and brominated polyphenylene ether resin, the phosphinates; Described fire retarding synergist comprises one or more in ANTIMONY TRIOXIDE SB 203 99.8 PCT, zinc borate, zinc, zinc oxide, sodium antimonate, boehmite, the tetrafluoroethylene; Described lubricant comprises one or more in lignite acid derivative, macromolecule wax class, low molecular weight liquid crystal polymkeric substance, metallic soap of stearic acid salt, stearic amide, the silicone compound; Described oxidation inhibitor comprises one or more in Hinered phenols antioxidant, suffocated amine antioxidant, phosphite ester kind antioxidant, thiodipropionate antioxidant or the thio-alcohol oxidation inhibitor.
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