CN112358713A - High-thermal-conductivity insulating PC/ABS composite material and preparation method thereof - Google Patents
High-thermal-conductivity insulating PC/ABS composite material and preparation method thereof Download PDFInfo
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Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L69/00—Compositions of polycarbonates; Compositions of derivatives of polycarbonates
-
- 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
-
- 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
- C08L2205/06—Polymer mixtures characterised by other features having improved processability or containing aids for moulding methods
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
The invention relates to a high-thermal-conductivity insulating PC/ABS composite material and a preparation method thereof. The high-thermal-conductivity insulation PC/ABS comprises PC, ABS, a toughening agent, a flaky thermal-conductivity insulation filler, a spherical thermal-conductivity insulation filler, a coupling agent, a main antioxidant, an auxiliary antioxidant and a lubricant, wherein the flaky thermal-conductivity insulation filler and the spherical thermal-conductivity insulation filler are respectively subjected to mixed acid treatment and coupling agent modification treatment in advance, then are subjected to blending melting extrusion with the ABS to prepare a thermal-conductivity insulation filler master batch, and then are compounded with other raw material components. The high-thermal-conductivity insulation PC/ABS composite material integrates the advantages of two resins, namely PC and ABS, so that the prepared composite material has high heat deformation temperature, high stability and high impact strength, and has rigidity, toughness and certain hardness; by using the flaky heat conduction insulating filler as the main filler and compounding the spherical heat conduction insulating filler, a multiple heat conduction network is constructed, the heat conduction efficiency of a system is effectively improved, and the heat conduction network has good insulating property.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a high-thermal-conductivity insulating PC/ABS composite material and a preparation method thereof.
Background
The heat conductivity coefficient of the plastic material is lower, generally below 0.3W/m.K, the failure of some plastic material products in the using process is caused by the fact that heat cannot be effectively dissipated and the working temperature is too high, in addition, along with the development of electronic components in the direction of high integration and small volume, the heat generated in the unit area is higher, the requirement of high heat conductivity is provided for the plastic material, so that the performance improvement of the plastic material in the aspect of heat conductivity can be better met, and the plastic material can be more effectively used for replacing steel.
The PC/ABS composite material effectively integrates the advantages of two resins, namely PC and ABS, is a composite material with the advantages of high impact strength, high processable flow property, high dimensional stability and the like, is widely applied to the fields of electronic and electric appliances, automobiles, communication and the like, and often has the requirement on heat dissipation in the fields. The heat conductivity coefficient of the PC/ABS can be effectively improved by adding the components such as graphite, carbon fiber, metal powder and the like, and the conductivity of the materials is also improved, but some products require the PC/ABS to have high heat dissipation performance and simultaneously retain the insulating characteristic of a plastic material, and the materials need to be modified in the aspects of heat conduction and insulation.
In the prior art, a technical scheme of modifying a plastic material in the aspects of heat conduction and insulation by adding insulating heat-conducting and insulating fillers such as aluminum oxide, aluminum nitride and BN is adopted, but the technical scheme needs a processing mode of firstly stirring and blending and then melting and granulating by an extruder, and as the heat-conducting and insulating inorganic fillers are generally powder with small particle size and have poor compatibility with the plastic material, the problems of difficult feeding, uneven blanking, agglomeration in the plastic and the like exist.
Disclosure of Invention
Accordingly, an object of the present invention is to provide a highly thermally conductive and insulating PC/ABS having advantages of excellent thermal conductivity, good dispersibility, and high interface strength.
A high-thermal-conductivity insulating PC/ABS composite material comprises the following raw material components in parts by weight:
the flaky heat-conducting insulating filler and the spherical heat-conducting insulating filler are respectively subjected to mixed acid treatment and coupling agent modification treatment in advance, then are subjected to blending, melting and extrusion with ABS to prepare heat-conducting insulating filler master batches, and then are compounded with other raw material components.
The high-thermal-conductivity insulating PC/ABS composite material provided by the embodiment of the invention integrates the advantages of two resins, namely PC and ABS, so that the prepared composite material has high thermal deformation temperature, high stability and high impact strength, and has rigidity, toughness and certain hardness; the composite material system has good insulating property by using the flaky heat conduction insulating filler as a main filler and compounding the spherical heat conduction insulating filler to construct a multiple heat conduction network, so that the heat conduction efficiency of the system is effectively improved, and the spherical heat conduction insulating filler is compounded for use; secondly, the embodiment of the invention effectively pretreats the flaky heat conduction insulating filler and the spherical heat conduction insulating filler, thereby greatly improving the compatibility of the flaky heat conduction insulating filler and a resin matrix, effectively solving the problem of difficult heat transfer caused by poor interface, further combining with the use of a toughening agent, improving the interface strength, effectively ensuring that the prepared composite material has higher impact strength, and being difficult to form cracks at the section so as to cause the problem of material fracture; in addition, the filler and the ABS are blended, melted and extruded to prepare the heat-conducting insulating filler master batch, and then the heat-conducting insulating filler master batch is compounded with other raw material components, so that the powdery heat-conducting insulating filler can be uniformly mixed with an ABS resin matrix, the dispersibility is good, the layering phenomenon or the agglomeration phenomenon cannot occur, and the problem of nonuniform blanking in the production process is solved.
Further, the PC is bisphenol A polycarbonate, is a non-crystalline engineering plastic with excellent comprehensive performance, is tasteless, odorless, nontoxic and high in transparency, has the advantages of excellent impact performance, size stability and the like, and is widely applied to the fields of optics, electronics, electricity, buildings and the like; the ABS is an acrylonitrile-butadiene-styrene terpolymer which has hardness, rigidity and toughness, is a general plastic with excellent non-crystalline comprehensive performance, is nontoxic and tasteless, can be formed by various processing modes, and has wide application in the fields of household appliances, automobiles, building materials and the like; the composite material prepared by blending PC and ABS has the advantages of PC and ABS, and the defects are mutually compensated, so that the composite material with extremely excellent comprehensive performance and wide application can be obtained.
Further, the flaky heat conducting and insulating filler has a particle size range of not more than 20 μm, is compounded with one or more selected from flaky BN, flaky AlN and flaky SiC, and has good heat conducting properties.
Further, the spherical heat-conducting insulating filler has a particle size range of not more than 20 μm, is compounded by one or more selected from spherical alumina, spherical BN and spherical SiC, and has good heat-conducting property and insulating property.
Further, the coupling agent is selected from one or more of a silane coupling agent KH540, a silane coupling agent KH550, a silane coupling agent K560, a titanate coupling agent NDZ101 and a titanate coupling agent NDZ102, and can effectively improve the compatibility of the filler and the resin matrix.
Further, the primary antioxidant is selected from hindered phenol antioxidants, and is selected from one or more of hindered phenol antioxidants 1010, 1076 and 245; the auxiliary antioxidant is selected from phosphite antioxidants, and is selected from one or more of phosphite antioxidant 168 and phosphite antioxidant PEP-36; the lubricant is selected from one or more of polyol ester lubricant, silicone lubricant and stearic acid lubricant. The use of the primary antioxidant and the secondary antioxidant can effectively inhibit the degradation of PC and ABS.
The high-thermal-conductivity insulating PC/ABS composite material provided by the embodiment of the invention integrates the advantages of two resins, namely PC and ABS, so that the prepared composite material has high thermal deformation temperature, high stability and high impact strength, and has rigidity, toughness and certain hardness; by using the flaky heat conduction and insulation filler as the main filler and compounding the spherical heat conduction and insulation filler, further in a preferred embodiment, the selection of the flaky heat conduction and insulation filler and the spherical heat conduction and insulation filler is limited, a multiple heat conduction network is constructed, the heat conduction efficiency of a system is effectively improved, and the composite material system has good insulation performance by combining the compounding use of the spherical heat conduction and insulation filler; secondly, the embodiment of the invention effectively pretreats the flaky heat conduction insulating filler and the spherical heat conduction insulating filler, thereby greatly improving the compatibility of the flaky heat conduction insulating filler and a resin matrix, effectively solving the problem of difficult heat transfer caused by poor interface, further combining the use of a toughening agent, and preferably selecting the toughening agent, so that the interface strength can be improved, and the prepared composite material is effectively ensured to have higher impact strength, and is not easy to form cracks at the section, thereby causing the problem of material fracture; in addition, the filler and the ABS are blended, melted and extruded to prepare the heat-conducting insulating filler master batch, and then the heat-conducting insulating filler master batch is compounded with other raw material components, so that the powdery heat-conducting insulating filler can be uniformly mixed with an ABS resin matrix, the dispersibility is good, the layering phenomenon or the agglomeration phenomenon cannot occur, and the problem of nonuniform blanking in the production process is solved.
In addition, the embodiment of the invention also provides a preparation method of the high-thermal-conductivity insulating PC/ABS composite material, which comprises the following specific operation steps:
1) respectively carrying out mixed acid treatment and coupling agent modification treatment on the flaky heat conduction insulating filler and the spherical heat conduction insulating filler;
2) and (2) treating the ABS and the heat-conducting insulating filler obtained in the step 1) after the mixed acid treatment and the coupling agent modification treatment according to the ratio of 20: 80-60: 40 parts by weight of the heat-conducting insulating filler master batch is uniformly mixed in mixing equipment, and after blending, the mixture is subjected to melt extrusion granulation through a stretching rheological extruder to prepare the heat-conducting insulating filler master batch;
3) weighing PC, ABS, a toughening agent, the heat-conducting insulating filler master batch obtained in the step 2), a coupling agent, a main antioxidant, an auxiliary antioxidant and a lubricant according to the ratio of the raw materials in the high-heat-conducting insulating PC/ABS composite material system, and adding the mixture into a blender for blending to obtain a premix;
4) and 3) melting, blending and extruding the premix obtained in the step 3) through an extruder to obtain the high-thermal-conductivity insulating PC/ABS composite material.
Further, the mixed acid treatment and the coupling agent modification treatment in the step 1) comprise the following treatment steps:
s1, preparing mixed acid solution, and adding concentrated H2SO4And concentrated HNO3According to the volume ratio of 1: 1-1: 3 uniformly mixing for later use; preparing a coupling agent solution, and mixing ethanol and deionized water according to a volume ratio of 80: 20-90: 10, uniformly mixing, then adding a coupling agent with a preset amount, continuously stirring under the conditions of condensation reflux and water bath heating, and uniformly mixing for later use;
s2, adding a flaky heat conduction insulating filler or a spherical heat conduction insulating filler into a reaction vessel, then adding the mixed acid solution obtained in the step S1, and uniformly mixing under the condition of mechanical stirring;
s3, performing ball milling treatment on the mixture obtained in the step S2;
s4, after the ball milling treatment is finished, centrifugally removing acid liquor after the obtained mixture is cooled to room temperature, washing the mixture for multiple times by using water until washing water is neutral, and drying the obtained solid to obtain primarily stripped and hydroxylated flaky heat-conducting insulating filler powder or spherical heat-conducting insulating filler powder;
s5, placing the flaky heat conduction insulating filler powder or the spherical heat conduction insulating filler powder obtained in the step S4 into a reaction container, adding the coupling agent solution obtained in the step S1, and carrying out mechanical stirring and ultrasonic treatment on the coupling agent solution;
s6, centrifugally filtering and drying the mixture obtained in the step S5 to obtain the active flaky heat conduction and insulation filler or spherical heat conduction and insulation filler which is subjected to mechanical stripping, acid mixing treatment and coupling agent modification treatment.
Further, the mixing equipment in the step 2) is an eccentric oscillation stirrer, the stirring speed in the mixing operation is 300-1500 rpm, and the problem of deposition and layering of the powdery filler can be effectively prevented in the eccentric oscillation process; when the extensional rheological extruder is used for extrusion granulation, the rotating speed of a main machine is 200-600 rpm, and the temperature of each zone is controlled to be 200-260 ℃;
the melt blending conditions of the extruder in the step 3) are as follows: firstly, stirring at a high speed of 2000-6000 rpm for 10-20 min, then stirring at a low speed of 200-2000 rpm for 1-6 min, and discharging at a rotating speed of 300-2000 rpm;
in the step 4), the rotation speed of a main machine is 200-600 rpm when the extruder is used for melt blending extrusion, and the temperature of each zone is controlled to be 210-260 ℃.
Further, in the step S3, the ball milling treatment is to put the mixture into a polytetrafluoroethylene ball mill pot, add a ball milling agent, and then install the mixture into a planetary ball mill for ball milling; the ball grinding agent is a zirconium ball, wherein the weight part ratio of the zirconium ball with the particle size of 20mm to the zirconium ball with the particle size of 10mm to the zirconium ball with the particle size of 6mm is 6: 80: 200 of a carrier; the ball milling procedure is in a bidirectional mode, the ball milling interval time is 1-5 min, the revolution speed of the ball mill is 20-200 rpm, and the rotation speed is 50-400 rpm.
In the preparation method of the high-thermal-conductivity insulating PC/ABS composite material, the flaky thermal-conductivity insulating filler and the spherical thermal-conductivity insulating filler are treated by using a mixed acid solution, hydrogen ions in the mixed acid solution are inserted between layered structures in filler molecules to cause the interlayer spacing to increase, meanwhile, hydroxyl groups can be introduced into the surface and the edge of the layered structures by the mixed acid to generate slight layered curling, the edge of the layered structures can be subjected to reactive cutting by the strong oxidation of the mixed acid, the effect of mechanical stripping of the filler structures is achieved by combining the extremely strong shearing force provided by revolution and autorotation of a ball milling tank in the ball milling process, and meanwhile, the hydroxylation of the surface of the filler can effectively increase the chemical active sites of the filler, thereby being beneficial to the modification of a subsequent coupling agent; in addition, in the ultrasonic treatment process, the energy provided by the ultrasonic can overcome the interlayer bonding force, the peeling of the flaky heat-conducting insulating filler is realized, and the re-agglomeration of the peeled nanosheet structure can be effectively avoided by mechanical stirring; meanwhile, after the coupling agent is combined with the hydroxyl grafted on the surface of the filler molecule, the surface polarity of the filler molecule is enhanced, and the dispersion of the filler molecule is further promoted, so that the stripping efficiency is greatly improved. The preparation method of the high-thermal-conductivity insulating PC/ABS composite material provided by the embodiment of the invention has the advantages of reasonable process design, good dispersion performance of the prepared composite material, simple preparation operation, low requirements on process and equipment, high production efficiency and low production cost, and is suitable for industrial large-scale production.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention more comprehensible, embodiments of the present invention are described in detail below.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways than those specifically described herein, and it will be apparent to those of ordinary skill in the art that the present invention may be practiced without departing from the spirit and scope of the present invention, and therefore the present invention is not limited by the examples disclosed below.
Example 1
The embodiment 1 of the invention provides a high-thermal-conductivity insulating PC/ABS composite material, which comprises the following raw materials in parts by weight: 80 parts of PC, 30 parts of ABS, 8 parts of MBS toughening agent, 18.8 parts of 10-micron sheet BN master batch, 6.3 parts of 15-micron spherical BN master batch, 1 part of coupling agent, 10105 parts of hindered phenol antioxidant, 1681 part of phosphite antioxidant and 3 parts of stearic acid lubricant.
Example 2
The embodiment 2 of the invention provides a high-thermal-conductivity insulating PC/ABS composite material, which comprises the following raw materials in parts by weight: 100 parts of PC, 50 parts of ABS, 10 parts of MBS toughening agent, 25 parts of 10-micron sheet BN master batch, 5 parts of 15-micron spherical BN master batch, 10 parts of coupling agent, 10105 parts of hindered phenol antioxidant, 1682 parts of phosphite antioxidant and 4 parts of polyol ester lubricant.
Example 3
The embodiment 3 of the invention provides a high-thermal-conductivity insulating PC/ABS composite material, which comprises the following raw materials in parts by weight: 150 parts of PC, 10 parts of ABS, 17 parts of MBS toughening agent, 30 parts of 10-micron sheet BN master batch, 2 parts of 15-micron spherical BN master batch, 5 parts of coupling agent, 10104 parts of hindered phenol antioxidant, 1682 parts of phosphite antioxidant and 2 parts of stearic acid lubricant.
Example 4
The embodiment 4 of the invention provides a high-thermal-conductivity insulating PC/ABS composite material, which comprises the following raw materials in parts by weight: 50 parts of PC, 100 parts of ABS, 13 parts of MBS toughening agent, 50 parts of 10-micron sheet BN master batch, 10 parts of 15-micron spherical BN master batch, 8 parts of coupling agent, 10104 parts of hindered phenol antioxidant, 1682 parts of phosphite antioxidant and 5 parts of stearic acid lubricant.
Example 5
The embodiment 5 of the invention provides a preparation method of a high-thermal-conductivity insulating PC/ABS composite material, which comprises the following specific operation steps:
1) respectively carrying out mixed acid treatment and coupling agent modification treatment on the flaky heat conduction insulating filler and the spherical heat conduction insulating filler;
specifically, the mixed acid treatment and the coupling agent modification treatment comprise the following specific operation steps:
s1, preparing mixed acid solution, and adding concentrated H2SO4And concentrated HNO3According to the volume ratio of 1: 1-1: 3 uniformly mixing for later use; preparing a coupling agent solution, and mixing ethanol and deionized water according to a volume ratio of 80: 20-90: 10, uniformly mixing, then adding a coupling agent with a preset amount, and stirring continuously under the conditions of condensation reflux and water bath heating, wherein the water bath heating temperature is 50-70 ℃, the stirring speed is 80-120 rpm, and mixingMixing uniformly for later use;
s2, adding a flaky heat conduction insulating filler or a spherical heat conduction insulating filler into a reaction vessel, then adding the mixed acid solution obtained in the step S1, and uniformly mixing under the condition of mechanical stirring;
s3, performing ball milling treatment on the mixture obtained in the step S2; in this embodiment, the mixture obtained in step S2 is distributed into a teflon ball mill, and after adding a ball milling agent, the mixture is ball milled in a planetary ball mill; the ball grinding agent is a zirconium ball, wherein the weight part ratio of the zirconium ball with the particle size of 20mm to the zirconium ball with the particle size of 10mm to the zirconium ball with the particle size of 6mm is 6: 80: 200 of a carrier; the ball milling procedure is in a bidirectional mode, the ball milling interval time is 1-5 min, the revolution speed of the ball mill is 20-200 rpm, and the rotation speed is 50-400 rpm;
s4, after the ball milling treatment is completed, cooling the obtained mixture to room temperature, centrifuging the mixture through a centrifuge to remove acid liquor, and washing the mixture for multiple times by using water until washing water is neutral, wherein the rotation speed condition of the centrifuge is 1800-2200 rpm; collecting the obtained solid in a drying disc, transferring the solid into a blast drying oven, and drying the solid for 2-4 hours at the temperature of 60-70 ℃ to obtain primarily stripped and hydroxylated flaky heat conduction and insulation filler powder or spherical heat conduction and insulation filler powder;
s5, placing the flaky heat conduction insulating filler powder or the spherical heat conduction insulating filler powder obtained in the step S4 into a reaction container, and adding the coupling agent solution obtained in the step S1, wherein the solid content of the coupling agent solution is 10% of that of the flaky heat conduction insulating filler powder, and carrying out mechanical stirring and ultrasonic treatment on the flaky heat conduction insulating filler powder for 4-12 hours, and the working power of an ultrasonic machine is 350-500W;
and S6, centrifugally filtering the mixture obtained in the step S5, collecting the mixture into a drying disc, transferring the mixture into a blast drying box, and drying the mixture for 2-6 hours at the temperature of 60-70 ℃ to obtain the movable flaky heat conduction insulating filler or spherical heat conduction insulating filler subjected to mechanical stripping, acid mixing treatment and coupling agent modification treatment.
2) And (2) treating the ABS and the heat-conducting insulating filler obtained in the step 1) after the mixed acid treatment and the coupling agent modification treatment according to the ratio of 20: 80-60: 40 parts by weight of the heat-conducting insulating filler master batch is uniformly mixed in mixing equipment, and after blending, the mixture is subjected to melt extrusion granulation through a stretching rheological extruder to prepare the heat-conducting insulating filler master batch; wherein the mixing equipment is an eccentric oscillation stirrer, and the stirring speed in the mixing operation is 300-1500 rpm; when the extensional rheological extruder is used for extrusion granulation, the rotating speed of a main machine is 200-600 rpm, and the temperature of each zone is controlled to be 200-260 ℃;
3) weighing PC, ABS, a toughening agent, the heat-conducting insulating filler master batch obtained in the step 2), a coupling agent, a main antioxidant, an auxiliary antioxidant and a lubricant according to the ratio of the raw materials in the high-heat-conducting insulating PC/ABS composite material system, and adding the mixture into a blender for blending to obtain a premix; wherein the extruder melt blending conditions are: firstly, stirring at a high speed of 2000-6000 rpm for 10-20 min, then stirring at a low speed of 200-2000 rpm for 1-6 min, and discharging at a rotating speed of 300-2000 rpm;
4) and (3) melting, blending and extruding the premix obtained in the step 3) through an extruder, wherein the rotating speed of a main machine is 200-600 rpm, and the temperature of each zone is controlled at 210-260 ℃, so that the high-thermal-conductivity insulating PC/ABS composite material is obtained.
Comparative example 1
Comparative example 1 provides a PC/ABS composite comprising the following raw materials in parts by weight: 80 parts of PC, 35 parts of ABS, 8 parts of MBS toughening agent, 10-micron spherical BN powder, 15-micron flaky BN powder, 1 part of coupling agent, 10104 parts of hindered phenol antioxidant, 1682 parts of phosphite antioxidant and 5 parts of stearic acid lubricant.
Comparative example 2
Comparative example 2 provides a PC/ABS composite comprising the following raw materials in parts by weight: 80 parts of PC, 35 parts of ABS, 8 parts of MBS toughening agent, 15-micron spherical BN powder, 15-micron flaky BN powder, 1 part of coupling agent, 10104 parts of hindered phenol antioxidant, 1683 parts of phosphite antioxidant and 4 parts of stearic acid lubricant.
Comparative example 3
Comparative example 3 provides a PC/ABS composite comprising the following raw materials in parts by weight: 100 parts of PC, 56 parts of ABS, 10 parts of MBS toughening agent, 10-micron sheet BN master batch, 5 parts of coupling agent, 10103 parts of hindered phenol antioxidant, 1684 parts of phosphite antioxidant and 2 parts of polyol ester lubricant.
Comparative example 4
Comparative example 4 provides a PC/ABS composite comprising the following raw materials in parts by weight: 100 parts of PC, 56 parts of ABS, 10 parts of MBS toughening agent, 15-micron spherical BN master batch, 5 parts of coupling agent, 10105 parts of hindered phenol antioxidant, 1683 parts of phosphite antioxidant and 5 parts of polyol ester lubricant.
The raw materials described in the above examples 1 to 4 and comparative examples 1 to 4 were prepared according to the preparation method described in example 5 to obtain the corresponding PC/ABS composite material, and the obtained PC/ABS material was sampled and tested, and the specific test data are shown in the following table:
first, it can be seen from the measured data that the surface resistivity of all samples was 1013And the voltage is higher than omega and is in an insulation level. The actual content of the heat-conducting insulating filler added in the embodiment 1 is the same as that of the heat-conducting insulating filler added in the comparative examples 1 and 2, and the difference is that the heat-conducting insulating filler in the embodiment 1 is subjected to surface chemical treatment and is simultaneously prepared into heat-conducting insulating filler master batches, so that the heat conductivity coefficient and the impact strength of the sample corresponding to the embodiment 1 are greatly higher than those of the samples corresponding to the comparative examples 1 and 2, which shows that the samples with high heat conductivity and high impact strength can be prepared only by pre-treating and mastered treating the heat-conducting insulating filler, and the good compatibility between the filler and a resin matrix is ensured, and the uniformity of feeding in the processing process is ensured; it can also be seen from comparative example 2 that, after the BN particle size exceeded 20 μm, although the thermal conductivity of the system increased, the impact strength decreased significantly because the larger the filler particle size, the less compatible with the matrix, and the more difficult it was to coat with the resin matrix. The difference between the example 2 and the comparative examples 3 and 4 is that the example 2 takes the flaky BN as the main heat-conducting network and is compounded with a small amount of spherical filler to improve the heat-conducting efficiencyThe proportion 3 has only added slice BN powder, and comparative example 4 has only added spherical BN powder, and the heat conduction effect of comparative example 4 is the worst, and the heat conduction effect of comparative example 3 is also obviously less than example 2, this is because slice BN constructs the heat conduction network effect and is obviously superior to spherical heat conduction insulating filler, but adds a small amount of spherical heat conduction insulating filler on slice heat conduction insulating filler basis and can produce the shape built effect, is favorable to further promoting the heat conduction effect.
Therefore, the high-thermal-conductivity insulation PC/ABS composite material provided by the embodiment of the invention integrates the advantages of two resins, namely PC and ABS, so that the prepared composite material has high heat deformation temperature, high stability and high impact strength, and has rigidity, toughness and certain hardness; by using the flaky heat conduction and insulation filler as the main filler and compounding the spherical heat conduction and insulation filler, further in a preferred embodiment, the selection of the flaky heat conduction and insulation filler and the spherical heat conduction and insulation filler is limited, a multiple heat conduction network is constructed, the heat conduction efficiency of a system is effectively improved, and the composite material system has good insulation performance by combining the compounding use of the spherical heat conduction and insulation filler; secondly, the embodiment of the invention effectively pretreats the flaky heat conduction insulating filler and the spherical heat conduction insulating filler, thereby greatly improving the compatibility of the flaky heat conduction insulating filler and a resin matrix, effectively solving the problem of difficult heat transfer caused by poor interface, further combining the use of a toughening agent, and preferably selecting the toughening agent, so that the interface strength can be improved, and the prepared composite material is effectively ensured to have higher impact strength, and is not easy to form cracks at the section, thereby causing the problem of material fracture; in addition, the filler and the ABS are blended, melted and extruded to prepare the heat-conducting insulating filler master batch, and then the heat-conducting insulating filler master batch is compounded with other raw material components, so that the powdery heat-conducting insulating filler can be uniformly mixed with an ABS resin matrix, the dispersibility is good, the layering phenomenon or the agglomeration phenomenon cannot occur, and the problem of nonuniform blanking in the production process is solved.
According to the preparation method of the high-thermal-conductivity insulating PC/ABS composite material, the flaky thermal-conductivity insulating filler and the spherical thermal-conductivity insulating filler are treated by using the mixed acid solution, hydrogen ions in the mixed acid solution are inserted between the layered structures in the filler molecules, so that the interlayer spacing is increased, meanwhile, hydroxyl groups can be introduced into the surface and the edge of the layered structures by the mixed acid, slight layered curling is generated, the edge of the layered structures can be cut in a reactive manner by the strong oxidation of the mixed acid, the effect of mechanical stripping of the filler structures is achieved by combining the extremely strong shearing force provided by revolution and rotation of a ball milling tank in the ball milling process, meanwhile, the chemical active sites of the filler surfaces can be effectively increased by hydroxylation of the filler surfaces, and subsequent modification of a coupling agent is facilitated; in addition, in the ultrasonic treatment process, the energy provided by the ultrasonic can overcome the interlayer bonding force, the peeling of the flaky heat-conducting insulating filler is realized, and the re-agglomeration of the peeled nanosheet structure can be effectively avoided by mechanical stirring; meanwhile, after the coupling agent is combined with the hydroxyl grafted on the surface of the filler molecule, the surface polarity of the filler molecule is enhanced, and the dispersion of the filler molecule is further promoted, so that the stripping efficiency is greatly improved. The preparation method of the high-thermal-conductivity insulating PC/ABS composite material provided by the embodiment of the invention has the advantages of reasonable process design, good dispersion performance of the prepared composite material, simple preparation operation, low requirements on process and equipment, high production efficiency and low production cost, and is suitable for industrial large-scale production.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention.
Claims (10)
1. The high-thermal-conductivity insulating PC/ABS composite material is characterized by comprising the following raw material components in parts by weight:
the flaky heat-conducting insulating filler and the spherical heat-conducting insulating filler are respectively subjected to mixed acid treatment and coupling agent modification treatment in advance, then are subjected to blending, melting and extrusion with ABS to prepare heat-conducting insulating filler master batches, and then are compounded with other raw material components.
2. The high thermal conductivity insulating PC/ABS composite of claim 1, wherein: the PC is bisphenol A polycarbonate; the ABS is acrylonitrile-butadiene-styrene terpolymer.
3. The high thermal conductivity insulating PC/ABS composite of claim 1, wherein: the particle size range of the flaky heat-conducting and insulating filler is not more than 20 mu m, and the flaky heat-conducting and insulating filler is compounded by one or more selected from flaky BN, flaky AlN and flaky SiC.
4. The high thermal conductivity insulating PC/ABS composite of claim 1, wherein: the spherical heat-conducting insulating filler has a particle size range of not more than 20 μm and is one or more selected from spherical alumina, spherical BN and spherical SiC.
5. The high thermal conductivity insulating PC/ABS composite of claim 1, wherein: the coupling agent is selected from one or more of a silane coupling agent KH540, a silane coupling agent KH550, a silane coupling agent K560, a titanate coupling agent NDZ101 and a titanate coupling agent NDZ 102.
6. The high thermal conductivity insulating PC/ABS composite of claim 1, wherein: the main antioxidant is selected from hindered phenol antioxidants, and is selected from one or more of hindered phenol antioxidants 1010, 1076 and 245; the auxiliary antioxidant is selected from phosphite antioxidants, and is selected from one or more of phosphite antioxidant 168 and phosphite antioxidant PEP-36; the lubricant is selected from one or more of polyol ester lubricant, silicone lubricant and stearic acid lubricant.
7. A preparation method of the high-thermal-conductivity insulating PC/ABS composite material as claimed in any one of claims 1 to 6, characterized by comprising the following specific operation steps:
1) respectively carrying out mixed acid treatment and coupling agent modification treatment on the flaky heat conduction insulating filler and the spherical heat conduction insulating filler;
2) and (2) treating the ABS and the heat-conducting insulating filler obtained in the step 1) after the mixed acid treatment and the coupling agent modification treatment according to the ratio of 20: 80-60: 40 parts by weight of the heat-conducting insulating filler master batch is uniformly mixed in mixing equipment, and after blending, the mixture is subjected to melt extrusion granulation through a stretching rheological extruder to prepare the heat-conducting insulating filler master batch;
3) weighing PC, ABS, a toughening agent, the heat-conducting insulating filler master batch obtained in the step 2), a coupling agent, a main antioxidant, an auxiliary antioxidant and a lubricant according to the ratio of the raw materials in the high-heat-conducting insulating PC/ABS composite material system, and adding the mixture into a blender for blending to obtain a premix;
4) and 3) melting, blending and extruding the premix obtained in the step 3) through an extruder to obtain the high-thermal-conductivity insulating PC/ABS composite material.
8. The preparation method of the high thermal conductivity insulation PC/ABS composite material according to claim 7, wherein the mixed acid treatment and the coupling agent modification treatment of step 1) comprise the following treatment steps:
s1, preparing mixed acid solution, and adding concentrated H2SO4And concentrated HNO3According to the volume ratio of 1: 1-1: 3 uniformly mixing for later use; preparing a coupling agent solution, and mixing ethanol and deionized water according to a volume ratio of 80: 20-90: 10, uniformly mixing, then adding a coupling agent with a preset amount, continuously stirring under the conditions of condensation reflux and water bath heating, and uniformly mixing for later use;
s2, adding a flaky heat conduction insulating filler or a spherical heat conduction insulating filler into a reaction vessel, then adding the mixed acid solution obtained in the step S1, and uniformly mixing under the condition of mechanical stirring;
s3, performing ball milling treatment on the mixture obtained in the step S2;
s4, after the ball milling treatment is finished, centrifugally removing acid liquor after the obtained mixture is cooled to room temperature, washing the mixture for multiple times by using water until washing water is neutral, and drying the obtained solid to obtain primarily stripped and hydroxylated flaky heat-conducting insulating filler powder or spherical heat-conducting insulating filler powder;
s5, placing the flaky heat conduction insulating filler powder or the spherical heat conduction insulating filler powder obtained in the step S4 into a reaction container, adding the coupling agent solution obtained in the step S1, and carrying out mechanical stirring and ultrasonic treatment on the coupling agent solution;
s6, centrifugally filtering and drying the mixture obtained in the step S5 to obtain the active flaky heat conduction and insulation filler or spherical heat conduction and insulation filler which is subjected to mechanical stripping, acid mixing treatment and coupling agent modification treatment.
9. The preparation method of the high thermal conductivity insulation PC/ABS composite material as claimed in claim 7, wherein the preparation method comprises the following steps:
the mixing equipment in the step 2) is an eccentric oscillation stirrer, and the stirring speed in the mixing operation is 300-1500 rpm; when the extensional rheological extruder is used for extrusion granulation, the rotating speed of a main machine is 200-600 rpm, and the temperature of each zone is controlled to be 200-260 ℃;
the melt blending conditions of the extruder in the step 3) are as follows: firstly, stirring at a high speed of 2000-6000 rpm for 10-20 min, then stirring at a low speed of 200-2000 rpm for 1-6 min, and discharging at a rotating speed of 300-2000 rpm;
in the step 4), the rotation speed of a main machine is 200-600 rpm when the extruder is used for melt blending extrusion, and the temperature of each zone is controlled to be 210-260 ℃.
10. The preparation method of the high thermal conductivity insulation PC/ABS composite material as claimed in claim 8, wherein:
the ball milling treatment in the step S3 is to place the mixture in a polytetrafluoroethylene ball milling tank, add a ball milling agent and then install the mixture in a planetary ball mill for ball milling; the ball grinding agent is a zirconium ball, wherein the weight part ratio of the zirconium ball with the particle size of 20mm to the zirconium ball with the particle size of 10mm to the zirconium ball with the particle size of 6mm is 6: 80: 200 of a carrier; the ball milling procedure is in a bidirectional mode, the ball milling interval time is 1-5 min, the revolution speed of the ball mill is 20-200 rpm, and the rotation speed is 50-400 rpm.
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