CN110564059A - high-thermal-conductivity polypropylene composite material and preparation method thereof - Google Patents
high-thermal-conductivity polypropylene composite material and preparation method thereof Download PDFInfo
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- 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
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/10—Homopolymers or copolymers of propene
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- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
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- C09K5/14—Solid materials, e.g. powdery or granular
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- C—CHEMISTRY; METALLURGY
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- 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
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- 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 belongs to the field of high-heat-conductivity materials, and particularly relates to a high-heat-conductivity polypropylene composite material and a preparation method thereof. The high-thermal-conductivity polypropylene composite material comprises the following raw materials in parts by weight: 80-100 parts of heat-conducting filler, 0-5 parts of chopped carbon fiber, 6-15 parts of modified polypropylene, 8-20 parts of high-strength polypropylene, 2-7 parts of high-fluidity polypropylene and an auxiliary agent. According to different proportions, the high-strength, high-fluidity and polarity modified polypropylene is adopted, and under the condition of adding 70-85% by mass of high powder of graphite and graphite flake, the polypropylene composite material is subjected to a second-order continuous extrusion composite granulation process, wherein the heat conductivity coefficient is 4-26W/m.k, the tensile strength is 15-30 MPa, the elongation at break is 3-5%, and the flow shear rate is 1-6, so that the heat-conducting composite material with high heat conductivity, high mechanical property and good processability is obtained.
Description
Technical Field
The invention belongs to the field of heat conduction materials, and particularly relates to a high-heat-conductivity polypropylene composite material and a preparation method thereof.
Background
Polypropylene is one of the substrates of high thermal conductivity materials in general, and its thermal conductivity is generally about 0.12W/(m · K). The production process of the high heat conductive polypropylene composite material is to add some heat conductive fillers (such as graphite, graphene, chopped carbon fiber, carbon black and the like), metal materials (copper, aluminum and the like) or metal oxide materials (aluminum hydroxide, magnesium hydroxide and the like) into a polypropylene matrix, and then to carry out mixing and single-stage extrusion granulation. The heat conduction material with the heat conduction coefficient of 2-4W/(m.K) is obtained, and the heat conduction requirement of the heat conduction polypropylene product is met.
In the polypropylene heat conduction material, the addition amount of the heat conduction filler is about 40-60%. If the amount is too low, the thermal conductivity cannot be satisfied, and if the amount is too high, the mechanical properties and the flow properties of the polypropylene product deteriorate, and the polypropylene product is difficult to mold and use. Therefore, if the heat-conducting filler is added in a high mass fraction (more than 70%), the mechanical properties of the material are poor (the tensile strength is generally less than 10MPa) and the reworking performance is extremely poor (the material has almost no flow property), so that the heat-conducting product (such as a heat exchanger and the like) can not be developed, and the use requirement of the mechanical properties of the product can not be met. Therefore, currently, the heat-conducting polypropylene material with the heat conductivity coefficient larger than 4W/m.k is really developed, has better mechanical property and processing property, and can develop industrial heat-conducting products for a few applications.
in addition, in the existing polypropylene heat conduction materials, only the heat conductivity or mechanical property of the material is mainly concerned, and the fluidity of the material is hardly considered, for example, in patent CN201711161110.6, 30-70 parts of a polypropylene composite material with a high heat conductivity coefficient is filled with 10-30 parts of modified glass fibers, wherein the melt index of polypropylene is limited to 10-25 g/10min, and although the heat conductivity can reach more than 4W/m.k, the mechanical property and the processing property of the material cannot meet the use requirements. In CN201310459396.1 reinforced polyolefin heat-conducting plastic and a preparation method thereof, the melt index of the copolymerized propylene is limited to 25-40 g/min, the notched impact strength of a cantilever beam is limited to 100-200J/m, and in order to improve the processability and mechanical property of heat conduction, the resin content is large, but the heat-conducting property can only reach 1.6W/m.k, but can not reach more than 4W/m.k. In the preparation method of CN201711098479.7 multi-element composite modified heat-conducting and electric-conducting polypropylene plastic and the product and application thereof, in order to solve the problems of high fluidity and high strength polypropylene performance, a large amount of polymer base material is added, and although the fluidity is improved, the heat-conducting performance is poor. If the specific gravity (more than 70%) of the heat-conducting filler is increased, the mechanical property and the flow property of the polymer support that the heat-conducting filler reaches the use standard, and the fluidity, the mechanical property and the heat conductivity cannot be simultaneously considered. In the CN201210319453.1 resin composition and the inverter element prepared from the same, the mass content of the added powder is 40-55%, the content of the resin base material is about 50%, the resin content is high, the processing performance requirement can be met, the effect of more than 4W/m.k can not be achieved under the formula, even if the carbon fiber with higher thermal conductivity coefficient is added, the thermal conductivity coefficient of more than 4W/m.k can not be achieved, the data in the table 2 obviously violates the scientific law and can not be used as the basis of the fact. In the CN201510040052.6 multifunctional polypropylene composite material and the preparation method thereof, the thermoplastic elastomer and the flexible fiber are added for toughening, so that the material is ensured to keep good mechanical property under the premise of high filling, the formula is complex, and the research on processing fluidity is not involved.
The heat-conducting polypropylene with the mass fraction of the heat-conducting powder being more than 70 percent has almost no flow property due to containing a large amount of powder, and the melt index cannot be detected, so that the processing is very difficult, even cannot be carried out. And the general polymer has good melt fluidity, low melt strength, large melt strength and poor fluidity. For example, high strength polypropylene (over 40 MPa) has poor flowability, the flow shear rate (melt flow rate) is only a few tenths to a few, which is not favorable for the mixing and melting and uniformity of the high filling material, and polypropylene with good flowability (MFR value is hundreds to thousands) has poor mechanical properties, very small tensile strength, and cannot achieve the mechanical properties required by the high filling material. And polypropylene is a non-polar material, and has poor miscibility with filler and interface performance. Therefore, the conventional polypropylene is selected as a base material of the high-heat-conduction material, and the high-heat-conduction material, the high-mechanical property and the good processability cannot be simultaneously met.
How to prepare the polypropylene high-heat-conduction material with the powder content of more than 70 percent, and the heat conduction performance is improved, and the processing flow performance and the mechanical performance of the polypropylene high-heat-conduction material can be ensured, which is a technical problem to be solved urgently at present.
Disclosure of Invention
In order to solve the problems of poor mechanical property and poor flow property of a high-heat-conductivity polypropylene material (the content of filler powder is more than 70%), the invention provides a high-heat-conductivity polypropylene composite material and a preparation method thereof.
The technical scheme adopted by the invention is specifically as follows:
The high-thermal-conductivity polypropylene composite material comprises the following raw materials in parts by weight:
further, the coupling agent is one selected from KH-550, KH-560 or KH-570; the antioxidant is one of antioxidant 1010, antioxidant 1098 and antioxidant 168; the flowing agent is ACR resin, such as one of ACR-201, ACR-301, and ACR-401.
The production process of the high-thermal-conductivity polypropylene composite material comprises the following steps:
(1) Carrying out surface treatment on graphite powder and graphite flakes by adopting a coupling agent to obtain modified graphite powder and graphite flakes for later use;
(2) Mixing modified graphite powder, graphite flakes, modified polypropylene, 0.5-1 part of a flow agent and 1-5 parts of high-fluidity polypropylene at a high speed to obtain a mixture 1;
(3) mixing high-strength polypropylene, chopped carbon fibers, 1-2 parts of high-fluidity polypropylene, 0.5-1 part of a flowing agent and an antioxidant at a high speed to obtain a mixture 2;
(4) second-order continuous extrusion composite granulation: and fully mixing and plasticizing the mixture 1 in a first-order double-screw extruder, controlling the temperature of a melt to be 180-250 ℃, mixing, then feeding the mixture into a feed inlet of a second-order double-screw extruder, simultaneously gradually feeding the mixture 2 into a feed inlet of the second-order extruder through a conveying device, fully plasticizing, mixing and melting the mixture 1 and the mixture 2 together in the second-order extruder, controlling the temperature of the melt to be 180-250 ℃, and granulating through a hot cutting unit to obtain the high-heat-conductivity polypropylene composite material.
Further, the graphite consists of 0-100 parts of graphite powder and 0-100 parts of graphite flakes, and the graphite powder and the graphite flakes jointly form 80-100 parts of heat conducting filler.
wherein the particle size of the graphite powder is 50-150 μm, the diameter of the graphite flake is 50-150 μm, and the thickness is 30-50 nm.
the heat conductivity coefficient of the graphite flake is as high as 1500W/(m.K), the heat conductivity is good, but the cost is high, so the invention mixes the graphite flake and the conventional heat-conducting graphite powder, which not only reduces the cost and is beneficial to controlling, but also is beneficial to improving the heat-conducting effect compared with single use because of the mutual cooperation of the graphite flake and the conventional heat-conducting graphite powder. Because the graphite powder is the likepowder, its heat conduction route that forms in the base member is through point contact formation, forms the contact space easily, is difficult for forming more heat circulation routes, and the graphite flake is a super flaky material, can pass through the lamella overlap joint in filling the base member, nevertheless because the size is little, the lamella is too thin, and the buildding between the lamella is not very regular. And with graphite powder and graphite flake used together, except that self contact is connected, there is contact heat flow path also between graphite flake and the graphite powder, and the space accessible graphite powder between two graphite flakes forms bridging formula heat flow network to can form more heat flow paths in the base member, more be favorable to the heat conduction effect to improve after cooperating.
And in the invention, chopped carbon fibers (the length is less than or equal to 3mm) are also added, the addition of the chopped carbon fibers is not only favorable for improving the mechanical strength of the polypropylene resin, but also has good heat-conducting property, can penetrate among resin groups, assists in constructing heat-conducting network structures among other graphite sheets in different forms and graphite powder fillers, and is favorable for further improving the heat-conducting property.
Further, the modified polypropylene is maleic anhydride grafted polypropylene resin;
the maleic anhydride grafted polypropylene resin is used for introducing polar groups into a nonpolar macromolecular skeleton of the polypropylene resin, so that the interfacial bonding force between the modified polypropylene resin and the modified heat-conducting filler is remarkably improved, and the mechanical property of the polypropylene heat-conducting material is improved.
The invention adopts a second-order continuous extrusion preparation method, and first, 70-85% of heat-conducting filler in mass fraction is fully mixed with maleic anhydride grafted polypropylene and part of high-fluidity polypropylene, so that the heat-conducting filler has full fluidity and strong interface bonding force. Then mixing with other materials to further improve the flow property and strength.
The invention adopts a second-order continuous extrusion method to separately mix materials with different functions, and the three acrylic resins have good compatibility, thereby being beneficial to improving the fluidity and the strength of the mixed materials and realizing the comprehensive modification of the product performance.
Further, the high-strength polypropylene is polypropylene with tensile strength close to or exceeding 40 MPa;
For example: northern Europe chemical engineering: RB707CF, nordic chemical: RD708CF, nordic chemical: BD212CF, majestic: HC9006BM and the like
Further, the high-fluidity polypropylene is polypropylene having a melt flow rate of 1000g/10min or more.
For example: ExxonMobil: achievee PP6936G2, ExxonMobil: PP3546G, ExxonMobil: PP3746G, and the like.
High-strength polypropylene, high-fluidity polypropylene and modified polypropylene are selected for blending, the compatibility of the three is good, various polypropylene chain segments are interacted and wound, the binding force is increased, mutual support and cooperation are realized, and the performance improvement is facilitated compared with single polypropylene. Thereby ensuring the mechanical property and the processing property of the high powder with the mass content of 70-85%.
Compared with the prior art, the invention has the beneficial effects that:
(1) The invention adopts the modified polypropylene with high strength, high fluidity and polarity to prepare the high-filling polypropylene heat conduction material according to different proportions, and obtains the heat conduction composite material with high heat conduction, high mechanical property and good processability. Under the condition of adding 70-85% of high powder by mass, the polypropylene composite material with the heat conductivity coefficient of 4-26W/m.k, the tensile strength of 15-30 MPa, the elongation at break of 3-5% and the flow shear rate of 1-6 can be obtained through a second-order continuous extrusion composite granulation process. The heat conduction material provides reliable heat conduction materials for developing products such as anticorrosive heat exchangers in the fields of chemical industry, environmental protection, mineral separation and the like, and meets the requirements of the market and the product design performance.
(2) The invention adopts the graphite, graphite flake and chopped carbon fiber with different heat conduction characteristics as heat conduction filler, and has synergistic effect, thereby reducing the cost and improving the heat conduction performance of the material.
(3) the second-order continuous extrusion composite granulation method disclosed by the invention is used for separately mixing materials with different functions, so that the fluidity and the strength of the mixed materials are better improved, and the comprehensive performance of the heat conduction material is improved.
Drawings
FIG. 1 is a flow chart of the present invention for preparing a high thermal conductivity polypropylene composite material by a second-order continuous extrusion method.
Detailed Description
example 1
The high-thermal-conductivity polypropylene composite material comprises the following raw materials in parts by weight:
(1) carrying out coupling agent surface treatment on the graphite powder and the graphite flake to obtain modified graphite powder and graphite flake;
(2) Mixing modified graphite powder, modified graphite flakes, maleic anhydride grafted polypropylene, 0.5 part of a flow agent and 5 parts of high-fluidity polypropylene at a high speed to obtain a mixture 1;
(3) mixing high-strength polypropylene, chopped carbon fibers, 2 parts of high-fluidity polypropylene, 0.5 part of a flow agent and an antioxidant at a high speed to obtain a mixture 2;
(4) Second-order continuous extrusion composite granulation: and fully mixing and plasticizing the mixture 1 in a first-order double-screw extruder, controlling the temperature of a melt to be 180-250 ℃, mixing, then feeding the mixture into a feed inlet of a second-order double-screw extruder, simultaneously gradually feeding the mixture 2 into a feed inlet of the second-order extruder through a conveying device, fully plasticizing, mixing and melting the mixture 1 and the mixture 2 together in the second-order extruder, controlling the temperature of the melt to be 180-250 ℃, and granulating through a hot cutting unit to obtain the high-heat-conductivity polypropylene composite material.
Example 2
And (3) performing second-order continuous extrusion composite granulation, wherein the preparation process is the same as that of example 1, so as to obtain the high-thermal-conductivity polypropylene composite material.
Example 3
And (3) performing second-order continuous extrusion composite granulation, wherein the preparation process is the same as that of example 1, so as to obtain the high-thermal-conductivity polypropylene composite material.
example 4
And (3) performing second-order continuous extrusion composite granulation, wherein the preparation process is the same as that of example 1, so as to obtain the high-thermal-conductivity polypropylene composite material.
Comparative examples 1 to 4
comparative example 1 and example 1; comparative example 2 and example 2; comparative example 3 compared to example 3; comparative example 4 differs from example 4 in that: the high-fluidity polypropylene was replaced with polypropylene having an MFR of 130g/10min, and the other ingredients and the preparation method were the same as in examples 1 to 4.
Wherein, the comparative example 1 has difficult processing in a double screw extruder and slow advancing speed, and the test results of the final product performance are shown in Table 2.
In contrast, in comparative examples 2 to 4, the powder content was too high (above 70%), which made the molding difficult, and the product could not be successfully processed for inspection.
Comparative examples 5 to 8
Comparative examples 5 to 8 are compared with examples 1 to 4, respectively, with the following differences: the high-fluidity polypropylene and the high-strength polypropylene were replaced with polypropylene having an MFR of 45g/min and a tensile strength of 30MPa (Nordic chemical: RS103SA), and the ingredients and the preparation method were the same as in examples 1 to 4.
of these, comparative example 5 was difficult to process in the twin-screw extruder and the advancing speed was slow, and the results of the performance tests obtained are shown in Table 2.
In comparative examples 6 to 8, the powder content was too high (above 70%), the molding was difficult, and the products could not be successfully processed for inspection.
comparative example 9
Comparative example 9 compared with example 1, the raw material components are the same, except that: and (3) adopting a single-stage double-screw extruder, putting all the raw materials into a mixer, fully mixing for twice the mixing time of the embodiment 3, adding the mixture into the double-screw extruder, fully mixing and plasticizing, and controlling the temperature to be 180-250 ℃. The materials are difficult to process in the double-screw extruder, the advancing speed is slow, the uniformity of the materials is poor, and the test results of the final product performance are shown in Table 2.
The polypropylene composite materials prepared in the above examples and comparative examples are respectively subjected to performance tests, and the detection results are shown in tables 1 and 2
TABLE 1
Table 2:
Claims (8)
1. A high heat conduction polypropylene composite material is characterized in that: the high-thermal-conductivity polypropylene composite material comprises the following raw materials in parts by weight:
2. The high thermal conductivity polypropylene composite material according to claim 1, wherein: the heat conducting filler consists of 0-100 parts of graphite powder and 0-100 parts of graphite flakes; wherein the particle size of the graphite powder is 50-150 μm, the diameter of the graphite flake is 50-150 μm, and the thickness of the graphite flake is 30-50 nm.
3. The high thermal conductivity polypropylene composite material according to claim 1, wherein: the modified polypropylene is maleic anhydride grafted polypropylene resin.
4. The high thermal conductivity polypropylene composite material according to claim 1, wherein: the high-flow polypropylene is polypropylene with the melt flow rate of more than 1000g/10 min.
5. The high thermal conductivity polypropylene composite material according to claim 1, wherein: the high-strength polypropylene is polypropylene with tensile strength of more than 40 MPa.
6. The high thermal conductivity polypropylene composite material according to claim 1, wherein: the coupling agent is one of KH-550, KH-560 or KH-570; the antioxidant is one of an antioxidant 1010, an antioxidant 1098 and an antioxidant 168; the flow agent is ACR resin.
7. The method for preparing a high thermal conductive polypropylene composite material according to any one of claims 1 to 6, wherein:
(1) Carrying out surface treatment on graphite powder and graphite flakes by adopting a coupling agent to obtain modified graphite powder and graphite flakes for later use;
(2) Mixing the modified graphite powder and the graphite flake with the modified polypropylene, the high-fluidity polypropylene and the flowing agent at a high speed to obtain a mixture 1;
(3) Mixing high-strength polypropylene, chopped carbon fibers, high-fluidity polypropylene, a flow agent and an antioxidant at a high speed to obtain a mixture 2;
(4) Second-order continuous extrusion composite granulation: and fully mixing and plasticizing the mixture 1 in a first-order double-screw extruder, feeding the mixture into a feed inlet of a second-order double-screw extruder after mixing, gradually feeding the mixture 2 into a feed inlet of the second-order extruder, fully plasticizing, mixing and melting the mixture 1 and the mixture 2 together in the second-order extruder, and granulating by a hot cutting unit to obtain the high-thermal-conductivity polypropylene composite material.
8. The preparation method of the high thermal conductivity polypropylene composite material according to claim 7, wherein: controlling the temperature of a melting material in a first-order double-screw extruder to be 180-250 ℃; the temperature of the melting material in the second-order screw extruder is controlled to be 180-250 ℃.
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| CN113831661A (en) * | 2020-06-24 | 2021-12-24 | 中国石油化工股份有限公司 | PVC protective fence composition for roads |
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