CN113861559B - Heat-conducting polypropylene material and preparation method and application thereof - Google Patents
Heat-conducting polypropylene material and preparation method and application thereof Download PDFInfo
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- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
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- C08K2003/222—Magnesia, i.e. magnesium oxide
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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Abstract
The invention discloses a heat-conducting polypropylene material, a preparation method and application thereof, wherein the heat-conducting polypropylene material comprises the following components in parts by weight: 60-83 parts of first polypropylene resin, 4-10 parts of second polypropylene resin, 2-10 parts of polyethylene resin, 1-5 parts of compatilizer, 3-8 parts of foam metal, 10-20 parts of heat conducting filler and 0.2-1 part of passivating agent. According to the invention, foam metal, heat conducting filler and melt-blown polypropylene are added simultaneously to modify the polypropylene material, and under the synergistic effect of the foam metal, the heat conducting filler and the melt-blown polypropylene, the heat conducting property of the material is greatly improved, the material is light, and meanwhile, the material has better electrical insulation property and mechanical property.
Description
Technical Field
The invention belongs to the technical field of modified plastics, and particularly relates to a heat-conducting polypropylene material, and a preparation method and application thereof.
Background
The heat conductive material has wide application in various fields of national defense industry and national economy, and the traditional heat conductive material is generally a metal material, but the application of the traditional heat conductive material is limited due to the poor corrosion resistance of the metal material. The polymer material has the characteristics of light weight, corrosion resistance, easy processing and forming, good electrical insulation performance, excellent mechanical property, fatigue resistance and the like, and plays an important role in the fields of information industry and the like at present. However, since most of the polymer materials are poor conductors and have extremely low thermal conductivity, for example, the thermal conductivity of polypropylene (PP) is only about 0.2W/(m·k), and the thermal conductivity of nylon 6 (PA 6) is only about 0.25W/(m·k). However, the thermal conductivity of the sheet is generally required to be 1.3 to 2W/(m·k) in the mechanical field, and is generally required to be 5W/(m·k) or more in the field of electronic products having an increasing chip content such as mobile phones.
In order to improve the thermal conductivity of the polymer material, the prior art generally adopts a method of adding metal oxide with better thermal conductivity, for example, CN112029275a discloses that the thermal conductivity of PA is improved by adding zinc oxide, magnesium oxide, aluminum oxide, boron nitride, zinc nitride, aluminum nitride, magnesium hydroxide, aluminum hydroxide, silicon carbide or graphite. However, this method results in a significant decrease in the mechanical properties of the material due to the excessive amount of heat transfer medium that needs to be added.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention aims to provide a heat-conducting polypropylene material and a preparation method and application thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
the heat-conducting polypropylene material comprises the following components in parts by weight: 60-83 parts of first polypropylene resin, 4-10 parts of second polypropylene resin, 2-10 parts of polyethylene resin, 1-5 parts of compatilizer, 3-8 parts of foam metal, 10-20 parts of heat conducting filler and 0.2-1 part of passivating agent.
Further, the first polypropylene resin is at least one of homo-polypropylene, co-polypropylene and random polypropylene, and the melt flow rate of the first polypropylene resin under the test condition of 230 ℃/2.16kg is 8-70 g/10min.
Further, the second polypropylene resin is melt-blown polypropylene, and the melt flow rate of the second polypropylene resin under the test condition of 230 ℃/2.16kg is 1200-2500 g/10min.
Preferably, the polyethylene resin is at least one of high density polyethylene, low density polyethylene, and linear low density polyethylene; in view of processability, it is more preferable to use linear low density polyethylene.
Preferably, the compatilizer is a graft modified polymer and comprises at least one of PP grafted maleic anhydride, POE grafted maleic anhydride and PP grafted dibutyl maleate.
Preferably, the foam metal is at least one of reduced iron powder and foam iron powder, but not limited to the two.
Preferably, the porosity of the foam metal is 60% -75%. The foam metal has too small porosity, is easy to collapse and is easy to conduct electricity; too much porosity may decrease the thermal conductivity.
Preferably, the heat conductive filler includes at least one of metal oxide (e.g., zinc oxide, magnesium oxide, etc.), metal hydroxide (e.g., aluminum hydroxide, magnesium hydroxide), etc.
Preferably, the weight ratio of the foam metal to the heat conducting filler is 0.2-0.5; more preferably 0.3 to 0.4. With the proportion, the polypropylene material has better comprehensive performance.
Preferably, the passivating agent is an antioxidant 1024. In general, the addition of metal components accelerates the degradation of the plastic, while the addition of the passivating agent prevents the metal from accelerating the degradation of the plastic.
Compared with heat conducting fillers such as metal oxides, metal hydroxides and the like, the foam metal used by the invention has higher electron conduction speed and higher heat conduction speed. Therefore, the addition of the foam metal can greatly improve the heat conduction performance of the polypropylene material, and can reduce the addition amount of the heat conduction filler in the polypropylene material, so that the material is light, and meanwhile, the influence of the low-ductility filler on the mechanical property of the material is reduced, so that the toughness of the material is better maintained. In addition, the foam metal has rigidity and toughness, so that the rigidity of the material is improved to a certain extent while the material has better toughness. However, if only a metal foam is added, the porous structure is broken, and the polypropylene material easily forms a conductive path. The existence of the heat conducting filler can form a certain barrier effect and improve the electrical insulation property of the polypropylene material, so that the effect of adding the foam metal and the heat conducting filler is better. Furthermore, the residual gaps of the foam metal can be completely filled by adding a proper amount of melt-blown polypropylene with the parameters, so that the heat conduction performance of the polypropylene material can be further improved, a more stable barrier effect can be formed, and the polypropylene material can be better prevented from forming a conductive path.
The polyethylene resin has low melting point and is easy to process, the polyethylene resin is used as auxiliary resin, the dispersibility of raw material components can be increased, the mechanical property of the polypropylene material is improved, particularly when the polypropylene material is prepared by a masterbatch method, the preparation of foam metal masterbatch by an internal mixer can be realized, the excessive extrusion of foam metal by a double-screw extruder is avoided, and the porous structure of the foam metal can be better reserved.
The invention also provides a preparation method of the heat-conducting polypropylene material, which comprises the following three steps:
method one (direct processing method): mixing the first polypropylene resin, the second polypropylene resin, the polyethylene resin, the compatilizer, the foam metal, the heat-conducting filler and the passivating agent, adding the mixture into a double-screw extruder for granulating, and cooling and blanking the mixture to obtain the heat-conducting polypropylene material.
Method two (half side feeding method): mixing the first polypropylene resin, the second polypropylene resin, the polyethylene resin, the compatilizer, the heat-conducting filler and the passivating agent, adding the mixture into a double-screw extruder for granulating, adding foam metal from a side feeding port, and cooling and blanking to obtain the heat-conducting polypropylene material. To better retain the metal foam structure, the side feed needs to be open at a position further back of the extruder to reduce the time the metal foam remains in the barrel.
Method three (masterbatch external mixing method): (1) Adding polyethylene resin, second polypropylene resin, compatilizer, foam metal and passivating agent into an internal mixer, heating and mixing, extruding and granulating by a single screw extruder to obtain foam metal master batch; (2) Mixing the first polypropylene resin and the heat-conducting filler, adding the mixture into a double-screw extruder for granulating, and cooling and blanking to obtain heat-conducting filler master batch; (3) And mixing the foam metal master batch and the heat-conducting filler master batch to obtain the heat-conducting polypropylene material which can be directly used for injection molding.
In the preparation method, the preparation method of the three master batches by an external mixing method is preferably adopted, the method can reduce the shearing of a screw on foam metal, better protect the porous structure of the foam metal, ensure that the electrical insulation property of the polypropylene material is better, ensure that the heat conductivity coefficient of the polypropylene material reaches more than 5W/(m.K), and meet the heat conductivity requirement of most electronic components.
The invention also provides application of the heat-conducting polypropylene material in preparing electronic components.
Compared with the prior art, the invention has the beneficial effects that: according to the invention, foam metal, heat conducting filler and melt-blown polypropylene are added simultaneously to modify the polypropylene material, so that under the synergistic effect of the foam metal, the heat conducting filler and the melt-blown polypropylene, the heat conducting property of the material is greatly improved, the material is light, and meanwhile, the material has excellent electrical insulation property and mechanical property, and has a good application prospect in the fields of electronic components and the like.
Detailed Description
The foregoing objects, features and advantages of the invention will be more readily apparent from the following detailed description of the embodiments. It will be apparent that the following examples are only some, but not all, of the examples of the invention. It should be understood that the embodiments of the present invention are only used for illustrating the technical effects of the present invention, and are not used for limiting the scope of the present invention. Unless otherwise indicated, all methods used in the examples of the present invention are conventional in the art, and the equipment, reagents, and starting materials used are commercially available.
The following raw materials used in the present invention are described below, but are not limited to these materials:
1. examples 1 to 6 and comparative examples 1 to 4 respectively provide a polypropylene material whose raw material formulation is shown in the following table 1:
TABLE 1
Note that: in the table "-" indicates that the component was not added.
The polypropylene materials of examples 1-6 were prepared using a half side feed method, as follows: mixing the other components except the foam iron powder or the reduced iron powder, adding the mixture into a double-screw extruder for granulation, and setting the foam iron powder or the reduced iron powder in a furnace of 40: and (3) adding the polypropylene material into a side feeding port at the 6 th section of the double-screw extruder, and cooling and cutting the polypropylene material. Wherein, the temperature of twin-screw extruder from first district to tenth district is in proper order: 160 ℃, 180 ℃, 190 ℃, 220 ℃, 230 ℃, 220 ℃, and 210 ℃.
The polypropylene materials of comparative examples 1 to 4 were prepared by referring to the preparation methods of examples 1 to 6.
In order to compare the influence of the preparation method on the material performance, the invention also adopts a direct processing method and a masterbatch external mixing method to prepare the polypropylene material according to the formula of the example 1.
The direct processing method comprises the following steps: according to the formulation of example 1, all the components were mixed, pelletized in a 40:1 twin screw extruder, cooled and cut to produce polypropylene material, designated product 2. Wherein, the temperature of twin-screw extruder from first district to tenth district is in proper order: 160 ℃, 180 ℃, 190 ℃, 220 ℃, 230 ℃, 220 ℃, and 210 ℃.
The masterbatch external mixing method comprises the following steps:
(1) Preparing foam metal master batches: adding polyethylene resin, second polypropylene resin, compatilizer, foam metal and passivating agent into an internal mixer, heating and mixing, extruding and granulating by a single screw extruder to obtain foam metal master batch; the process condition of the internal mixer is 170 ℃, the internal mixing is carried out for 10-15 min, and extrusion granulation is carried out for 2-3 min after the current is stabilized; the temperature of the single screw extruder from the first zone to the sixth zone was 170 ℃, 180 ℃ and 170 ℃ in that order;
(2) Preparing heat conducting filler master batch: mixing the first polypropylene resin and the heat-conducting filler, adding the mixture into a double-screw extruder for granulating, and cooling and blanking to obtain heat-conducting filler master batch; the temperatures of the twin-screw extruder from the first zone to the tenth zone were in order: 170 ℃, 190 ℃, 220 ℃, 240 ℃, 250 ℃, 240 ℃ and 220 ℃;
(3) And mixing the foam metal master batch and the heat-conducting filler master batch to obtain the polypropylene material which can be directly used for injection molding, and marking the polypropylene material as a product 3.
The formulation of example 1 was prepared using a semi-side feed process to produce a polypropylene material designated product 1.
Performance testing
The polypropylene materials prepared in the above examples and comparative examples were subjected to performance testing, and the relevant performance testing criteria or methods were as follows:
tensile strength: dumbbell type sample bars meet GB/T1040.1-2006;
impact strength: injection molding a notch spline, wherein the notch is A-shaped and meets GB/T1843-2008;
thermal conductivity coefficient: 100mm multiplied by 3mm square plates, which meet GB/T10294-2008;
surface resistance: 100mm multiplied by 3mm square plates, which meet GB/T1410-2006;
density: and the impact spline test is adopted, so that GB/T1033-2008 is satisfied.
The test results are shown in table 2:
TABLE 2
Note that: when the heat conductivity coefficient reaches more than 5W/(m.K), the electronic product with the increasingly increased chip content such as the mobile phone can meet the heat conductivity requirement; the surface resistance reaches 1X 10 6 Above Ohm, the use safety is better, otherwise the conductive path is easy to form, and the electronic component is broken down.
Analysis of results: from the products 1 to 3 in example 1, it can be seen that the difference of the properties of the prepared polypropylene materials is caused by the difference of the preparation methods, and the material is prepared by the masterbatch external mixing method, while the material improves the heat conductivity, the surface resistance is maximum, the electrical insulation property is optimal, and the mechanical property and the heat conduction property can meet the application requirements of electronic components, so that the masterbatch external mixing method is preferably adopted for preparation. Between the product 1 of example 1 and examples 2 to 3, example 2 was the preferred formulation for example 2, since it was optimal in terms of both heat conduction and electrical insulation properties, and also good in mechanical properties. Comparing product 1 with example 4, it is known that the difference of the types of the first polypropylene resins also affects the mechanical properties and the electrical insulation properties of the material, which depend on the characteristics of the first polypropylene resin itself, so that different types of the first polypropylene resins can be selected according to the performance requirements of the product and applied to different products. It can be seen from comparative examples 1 to 4 that only when the polypropylene material is modified by adding foam metal, heat conducting filler and melt-blown polypropylene, the material can simultaneously give consideration to heat conducting property and electrical insulating property, and mechanical property can be improved to a certain extent. It can also be seen from the product 1 and the comparative example 3 that the density of the material can be reduced by replacing part of the heat conductive filler with foam metal, so that the weight of the material can be reduced. It is also seen from example 6 that example 6 uses the foam iron powder B having a low porosity (50%), resulting in a decrease in the surface resistance of the material and a decrease in the electrical insulation property.
2. In order to explore the influence of the ratio of foam metal to heat conducting filler on the performance of polypropylene materials, test groups 1-4 of Table 3 were designed, wherein the foam metal used was foam iron powder, and the heat conducting filler used was formed by mixing zinc oxide and aluminum hydroxide in a weight ratio of 1:1. The PP materials are prepared from the test groups 1 to 4 by a half-side feeding method according to the formula of the example 2, wherein the total addition amount of the foam iron powder and the heat conducting filler is 22 parts, and the types and the addition amounts of other components are the same as those of the example 2.
TABLE 3 Table 3
| Group of | Foam metal heat conductive filler (weight ratio) |
| Test group 1 | 0.2 |
| Test group 2 | 0.3 |
| Test group 3 | 0.4 |
| Test group 4 | 0.5 |
The performance of the PP material prepared above was tested and the results are shown in table 4:
TABLE 4 Table 4
As can be seen from the data in the table, as the content ratio of the foam metal increases, the heat conductivity coefficient of the material gradually increases, but the surface resistance also gradually decreases; when the weight ratio of the foam metal to the heat conducting filler is 0.2-0.5, the heat conducting property, the electrical insulation property and the mechanical property of the material can all meet the use requirements of most electronic components, and particularly when the weight ratio of the foam metal to the heat conducting filler is 0.3-0.4, the heat conducting property and the electrical insulation property of the material can be well balanced.
Finally, it should be noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made to the technical solution of the present invention without departing from the spirit and scope of the technical solution of the present invention.
Claims (5)
1. The heat-conducting polypropylene material is characterized by comprising the following components in parts by weight: 60-83 parts of first polypropylene resin, 4-10 parts of second polypropylene resin, 2-10 parts of polyethylene resin, 1-5 parts of compatilizer, 3-8 parts of foam metal, 10-20 parts of heat conducting filler and 0.2-1 part of passivating agent, wherein the first polypropylene resin is at least one of homo-polypropylene, co-polypropylene and random polypropylene, the melt flow rate of the first polypropylene resin under the test condition of 230 ℃/2.16kg is 8-70 g/10min, the second polypropylene resin is melt-blown polypropylene, and the melt flow rate of the second polypropylene resin under the test condition of 230 ℃/2.16kg is 1200-2500 g/10min;
the foam metal is at least one of reduced iron powder and foam iron powder;
the heat-conducting filler comprises at least one of metal oxide and metal hydroxide;
the porosity of the foam metal is 60% -75%;
the weight ratio of the foam metal to the heat conducting filler is 0.2-0.5;
the passivating agent is an antioxidant 1024.
2. The thermally conductive polypropylene material of claim 1, wherein the polyethylene resin is at least one of high density polyethylene, low density polyethylene, and linear low density polyethylene.
3. The thermally conductive polypropylene material of claim 1, wherein the compatibilizer is a graft modified polymer comprising at least one of PP grafted maleic anhydride, POE grafted maleic anhydride, PP grafted dibutyl maleate.
4. A method for preparing a heat conductive polypropylene material according to any one of claims 1 to 3, comprising the steps of:
mixing the first polypropylene resin, the second polypropylene resin, the polyethylene resin, the compatilizer, the foam metal, the heat-conducting filler and the passivating agent, adding the mixture into a double-screw extruder for granulation, and cooling and blanking to prepare the heat-conducting polypropylene material;
or mixing the first polypropylene resin, the second polypropylene resin, the polyethylene resin, the compatilizer, the heat-conducting filler and the passivating agent, adding into a double-screw extruder for granulating, adding foam metal from a side feeding port, and cooling and cutting to obtain the heat-conducting polypropylene material;
or (1) adding polyethylene resin, second polypropylene resin, compatilizer, foam metal and passivating agent into an internal mixer, heating and mixing, extruding and granulating by a single screw extruder to obtain foam metal master batches; (2) Mixing the first polypropylene resin and the heat-conducting filler, adding the mixture into a double-screw extruder for granulating, and cooling and blanking to obtain heat-conducting filler master batch; (3) And mixing the foam metal master batch and the heat-conducting filler master batch to obtain the heat-conducting polypropylene material which can be directly used for injection molding.
5. The use of a thermally conductive polypropylene material as claimed in any one of claims 1 to 3 in the manufacture of electronic components.
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| CN109943023A (en) * | 2019-04-08 | 2019-06-28 | 深圳先进技术研究院 | A kind of thermally conductive electromagnetic shielding composite material and its preparation method and application |
| CN112662061A (en) * | 2020-12-18 | 2021-04-16 | 广东金发科技有限公司 | Low-shrinkage modified polypropylene resin and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109943023A (en) * | 2019-04-08 | 2019-06-28 | 深圳先进技术研究院 | A kind of thermally conductive electromagnetic shielding composite material and its preparation method and application |
| CN112662061A (en) * | 2020-12-18 | 2021-04-16 | 广东金发科技有限公司 | Low-shrinkage modified polypropylene resin and preparation method and application thereof |
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