CN112852138A - Thermoplastic resin-based conductive composite material and preparation method thereof - Google Patents
Thermoplastic resin-based conductive composite material and preparation method thereof Download PDFInfo
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Abstract
The application relates to the technical field of engineering plastics, and provides a thermoplastic resin-based conductive composite material and a preparation method thereof. The thermoplastic resin-based conductive composite material comprises the following components in parts by weight: 98.6-67 parts of thermoplastic resin; 1-15 parts of carbon nanotubes; 0-6 parts of a compatilizer; 0-5 parts of a nucleating agent; 0.2-1 part of antioxidant; 0-2 parts of a coupling agent; and 0.2-4 parts of other auxiliary agents, wherein the content of the compatilizer, the content of the nucleating agent and the content of the coupling agent are not 0. The thermoplastic resin-based conductive composite material provided by the application has excellent mechanical properties and processability, and simultaneously has the advantage of low volume resistivity.
Description
Technical Field
The application belongs to the technical field of engineering plastics, and particularly relates to a thermoplastic resin-based conductive composite material and a preparation method thereof.
Background
Thermoplastics are a class of plastics that are plastic at a certain temperature, solidify upon cooling, and repeat this process. The thermoplastic plastic has excellent mechanical property, wear resistance, dimensional stability, chemical corrosion resistance and the like, and can be widely applied to the fields of textile machinery, plastics, food, electronics, electricity, automobiles, light industry, chemical industry, buildings and the like. In the field of conductivity/antistatic property of thermoplastic plastics, at present, conductive carbon black powder and carbon fibers are mainly added into a thermoplastic plastic base material to enhance the conductivity and antistatic property of a product. When the carbon fiber is added as the conductive agent, although the addition amount of the carbon fiber is small, the carbon fiber is high-modulus fiber, so that obvious floating fiber can be generated on the surface of the material, and more additives are required to be added in the processing process to improve the compatibility of the carbon fiber and resin so as to improve the phenomenon of floating fiber, so that the production cost is increased, and the mechanical property of the material is influenced; meanwhile, the problem of fiber floating needs to be improved by proper forming process conditions, which undoubtedly increases the cost and conditions of processing and forming. When the conductive carbon black is added as a conductive agent, if the composite material is required to have lower volume resistivity, the addition amount of the conductive carbon black powder is larger (10 wt% -20 wt%). The addition of excessive conductive carbon black powder can cause the disadvantages of poor toughness and low impact strength of the material.
Disclosure of Invention
Problems to be solved by the invention
The application aims to provide a thermoplastic resin-based conductive composite material and a preparation method thereof, and aims to solve the problems that the volume resistivity and the processing forming of the existing thermoplastic material are simple, and the toughness and the impact strength of the material cannot be considered at the same time.
Means for solving the problems
In order to achieve the purpose of the application, the technical scheme adopted by the application is as follows:
the application provides a thermoplastic resin-based conductive composite material in a first aspect, which comprises the following components in parts by weight:
wherein the content of the compatilizer, the nucleating agent and the coupling agent is not 0.
Preferably, the nucleating agent is selected from one or more of silicate, stearate, nano-montmorillonite, carbon powder, zinc powder, barium sulfate, mica powder, talcum powder, zinc oxide, carbonate, phosphate, sodium benzoate, monocarboxylate, benzoate, aromatic phosphate, aromatic sulfonate, polyethylene glycol diglycidyl ether, glycidyl methacrylate copolymer, polyolefin, polytetrafluoroethylene, ethylene-acrylic acid copolymer salt, polypentylene glycol dibenzoate, triphenyl phosphate, phthalate and amide ester.
Preferably, the grain diameter of the nucleating agent is 1-10 μm.
Preferably, the total weight of the thermoplastic resin and the carbon nanotubes is 80-95% based on 100% of the total weight of the thermoplastic resin-based conductive composite material.
Preferably, the thermoplastic resin is selected from one or more of PP, PE, AS, ABS, PS, PC, nylon, polyester, PPO, PPS, POM, POK, LCP and HIPS.
Preferably, the compatilizer is one or more selected from maleic anhydride grafted polyolefin elastomer, acrylate-glycidyl ester-ethylene copolymer, methacrylate-styrene butadiene rubber-styrene copolymer, ethylene-acrylate copolymer, ethylene-vinyl acetate copolymer, acrylonitrile-butadiene-styrene copolymer, acrylonitrile-ethylene-styrene copolymer and block copolymer containing a polyester hard segment and a polyether soft segment.
Preferably, the coupling agent is one or more of silanes, titanates, aluminates and phosphates.
Preferably, the antioxidant is selected from one or more of 1010, 1098, 1076, 3114, 168, 626, 627A and 9228.
Preferably, the other auxiliary agents are selected from one or more of conventional additives such as ultraviolet absorbers, colorants, lubricants, mold release agents, silicone oil and white mineral oil.
The second aspect of the application provides a preparation method of a thermoplastic resin-based conductive composite material, which comprises the following steps:
weighing the raw material components according to the ligand of the thermoplastic resin-based conductive composite material in the first aspect;
drying the thermoplastic resin-based conductive composite material for 0-4 hours at the temperature of 80-140 ℃;
respectively adding the dried thermoplastic resin, the compatilizer, the nucleating agent, the antioxidant, other auxiliaries and the coupling agent into a stirrer, and stirring and mixing for 3-5 minutes at the rotating speed of 200-500 rpm to obtain a uniformly mixed premix;
adding carbon nanotubes into the premix, and stirring and mixing for 3-5 minutes at a rotating speed of 200-500 rpm to obtain a mixture;
and adding the mixture into a double-screw extruder, and performing melt extrusion granulation, water cooling, air drying, grain cutting and drying to obtain the thermoplastic resin-based conductive composite material.
Preferably, in the step of adding the mixture into the twin-screw extruder, the screw rotation speed is 400-900 rpm.
Effects of the invention
On one hand, the thermoplastic resin-based conductive composite material provided by the application takes the carbon nanotubes as the only conductive agent of the composite material, reduces the molecular interfacial force between the carbon nanotubes by the nucleating agent, destroys the combination between the carbon nanotubes, realizes the mutual dispersion of the carbon nanotubes, and further uniformly disperses in thermoplastic resin under the action of other auxiliary components such as compatilizers and coupling agents to construct a conductive network structure and play a good conductive role; on the other hand, the nucleating agent can accelerate the crystallization speed of the thermoplastic resin and refine the crystal grain structure, which is undoubtedly beneficial to shortening the molding period and improving the impact strength of the product and the dimensional stability of the final product, the carbon nano tube can also obviously improve the mechanical property of the thermoplastic resin, the nucleating agent and the carbon nano tube play a synergistic role in the thermoplastic resin, and the two components are added to promote the improvement of the comprehensive performance of the thermoplastic resin-based conductive composite material. The thermoplastic resin-based conductive composite material provided by the application has low volume resistivity and can keep good mechanical properties.
According to the preparation method of the thermoplastic resin-based conductive composite material, the thermoplastic resin is subjected to preheating treatment to remove moisture of the thermoplastic resin, so that the bonding force of a premix obtained by mixing the thermoplastic resin and the components except the carbon nano tubes is weakened, the carbon nano tubes can be endowed with good dispersibility in the step of adding the carbon nano tubes, and then the carbon nano tubes are uniformly dispersed in the thermoplastic resin with the help of the nucleating agent and other auxiliary components, so that the better mechanical property and the lower volume resistivity are realized.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects to be solved by the present application more clearly apparent, the present application is further described in detail below with reference to the embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the present application and are not intended to limit the present application.
In this application, the term "and/or" describes an association relationship of associated objects, meaning that there may be three relationships, e.g., a and/or B, which may mean: a is present alone, A and B are present simultaneously, and B is present alone. Wherein A and B can be singular or plural. The character "/" generally indicates that the former and latter associated objects are in an "or" relationship.
In the present application, "at least one" means one or more, "several" means two or more. "at least one of the following" or similar expressions refer to any combination of these items, including any combination of the singular or plural items. For example, "at least one (a), b, or c", or "at least one (a), b, and c", may each represent: a, b, c, a-b (i.e., a and b), a-c, b-c, or a-b-c, wherein a, b, and c may be single or plural, respectively.
It should be understood that, in various embodiments of the present application, the sequence numbers of the above-mentioned processes do not mean the execution sequence, some or all of the steps may be executed in parallel or executed sequentially, and the execution sequence of each process should be determined by its function and inherent logic, and should not constitute any limitation to the implementation process of the embodiments of the present application.
The terminology used in the embodiments of the present application is for the purpose of describing particular embodiments only and is not intended to be limiting of the application. As used in the examples of this application and the appended claims, the singular forms "a", "an", and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise.
The terms "first" and "second" are used for descriptive purposes only and are used for distinguishing purposes such as substances from one another, and are not to be construed as indicating or implying relative importance or implying any number of technical features indicated. For example, a first XX may also be referred to as a second XX, and similarly, a second XX may also be referred to as a first XX, without departing from the scope of embodiments of the present application. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature.
The weight of the related components mentioned in the description of the embodiments of the present application may not only refer to the specific content of each component, but also represent the proportional relationship of the weight among the components, and therefore, the content of the related components is scaled up or down within the scope disclosed in the description of the embodiments of the present application as long as it is scaled up or down according to the description of the embodiments of the present application. Specifically, the mass may be a unit mass known in the chemical industry, such as μ g, mg, g, kg, ton, etc.
The term "PP" is "polypropylene", meaning polypropylene;
the term "PE" is an abbreviation for "polyethylene", which means polyethylene;
the term "AS" is an abbreviation for "acrylonitril-styrene copolymer", which means an acrylonitrile-styrene copolymer;
the term "ABS" is an abbreviation for "Acrylonitrile Butadiene Styrene," which means Acrylonitrile-Butadiene-Styrene copolymer;
the term "PS" is an abbreviation for "Polystyrene", which stands for Polystyrene;
the term "PC" denotes polycarbonate;
the term "PPO" is an abbreviation for "PolyphenyleneOxide", which means polyphenylene oxide or ether;
the term "PPS" is an abbreviation for "Polyphenylene sulfide", which means Polyphenylene sulfide;
the term "POM" is an abbreviation for "polyoxymethylene (polyformaldehyde)", which means a polyoxymethylene resin;
the term "POK" is a polyketone material, and is a novel green polymer material formed by polymerizing CO, ethylene and propylene;
the term "LCP" is an abbreviation for "Liquid Crystal polymer" and denotes Liquid Crystal polymers.
The term "HIPS" is an abbreviation for "High Impact Polystyrene" and denotes High Impact Polystyrene.
The carbon nano tube is a one-dimensional quantum material, and a coaxial seamless nano-scale hollow circular tube with several layers to tens of layers is formed by carbon atoms formed by arranging hexagonal grids of single-layer or multi-layer graphite sheets. The carbon nano tube has extremely large specific surface area, electrical conductivity three orders of magnitude higher than that of metallic copper, high thermal conductivity 5 times higher than that of the metallic copper, larger length-diameter ratio, high tensile/bending strength (superior to any current fiber material), high thermal stability, excellent corrosion resistance, high elasticity, low density and the like. Due to the unique characteristics of the carbon nano tube, the carbon nano tube becomes a multifunctional material and a multifunctional structural material, and is expected to be applied to multiple aspects of electric conduction, heat conduction, high strength and the like in the field of materials. In view of this, it is preferable that,
on one hand, the embodiment of the application provides a thermoplastic resin-based conductive composite material, which comprises the following components in parts by weight:
wherein the content of the compatilizer, the nucleating agent and the coupling agent is not 0.
On one hand, the thermoplastic resin-based conductive composite material provided by the embodiment of the application takes the carbon nanotubes as the only conductive agent of the composite material, reduces the molecular interfacial force between the carbon nanotubes by the nucleating agent, destroys the combination between the carbon nanotubes, realizes the mutual dispersion of the carbon nanotubes, and further uniformly disperses the carbon nanotubes in the thermoplastic resin under the action of other auxiliary components such as a compatilizer and a coupling agent to construct a conductive network structure, thereby playing a good conductive role; on the other hand, the nucleating agent can accelerate the crystallization speed of the thermoplastic resin and refine the crystal grain structure, which is undoubtedly beneficial to shortening the molding period and improving the impact strength of the product and the dimensional stability of the final product, the carbon nano tube can also obviously improve the mechanical property of the thermoplastic resin, the nucleating agent and the carbon nano tube play a synergistic role in the thermoplastic resin, and the two components are added to promote the improvement of the comprehensive performance of the thermoplastic resin-based conductive composite material. The thermoplastic resin-based conductive composite material provided by the application has low volume resistivity and can keep good mechanical properties.
Specifically, the thermoplastic resin is used as a matrix component of the composite material in the embodiments of the present application, so that the composite material can exert the physical and chemical functions of the thermoplastic resin, such as the properties of softening by heating and hardening by cooling, good mechanical properties, and the like. In some embodiments, the thermoplastic resin is selected from one or more of PP, PE, AS, ABS, PS, PC, nylons, polyesters, PPO, PPs, POM, POK, LCP, HIPS. In the examples of the present application, the parts of the thermoplastic resin as the matrix component of the composite material are 98.6 to 67 parts, and the parts of the thermoplastic resin are, for example, 98.6 parts, 95 parts, 90 parts, 85 parts, 80 parts, 75 parts, 70 parts, 67 parts, and the like, based on 100 parts of the total weight of the composite material, but are not limited thereto.
In the embodiment of the application, the carbon nanotube is used as a conductive component of the composite material, and the carbon nanotube is the only conductive component of the composite material. After the carbon nano tubes are uniformly dispersed in the thermoplastic resin, the conductivity of the composite material can be effectively improved, so that the volume resistivity of the composite material is reduced. Compared with the method that the conductive carbon black is used as a conductive agent, the carbon nano tube can form a good conductive network structure in the thermoplastic resin matrix after being used as the conductive agent, and the obtained thermoplastic resin-based conductive composite material can keep good mechanical properties; compare and adopt the combined material that contains the carbon fiber as the conducting agent, the thermoplastic resin base conductive composite behind the carbon nanotube as the conducting agent, not only can not produce and float the fibre, improve processing convenience, the processing degree of difficulty and cost have been reduced, but also can not need to build the conductive network with the help of other conductive component (if in some technologies, on the basis of carbon fiber as conductive main part composition, through adding carbon nanotube or conductive carbon black as supplementary conductive component, when solving the carbon fiber of independent use as conductive network, the too big problem of the conductivity difference of goods surface different positions). The carbon nanotubes used in the embodiments of the present application may be single-walled carbon nanotubes or multi-walled carbon nanotubes.
In the embodiment of the application, the carbon nanotube is 1-15 parts by weight based on 100 parts by weight of the composite material. The parts of the carbon nanotubes are exemplified by specific parts such as 1 part, 2 parts, 3 parts, 4 parts, 5 parts, 6 parts, 7 parts, 8 parts, 9 parts, 10 parts, 12 parts, 15 parts, etc., but are not limited thereto. In some embodiments, after the carbon nanotubes are uniformly dispersed, a better conductive effect can be achieved with a smaller addition amount, so that the volume resistivity of the composite material is reduced. In some embodiments, the portion of carbon nanotubes is less than 10 parts based on 100 parts total weight of the composite.
In the embodiment of the application, the dispersion of the carbon nanotubes directly affects the level of the conductive performance of the composite material. The carbon nano tube has good dispersibility in the thermoplastic resin, so that the electrical conductivity of the composite material is improved, and the volume resistivity is reduced; however, when the dispersibility of the carbon nanotubes in the thermoplastic resin is deteriorated, the carbon nanotubes cannot exhibit a good conductive effect, but the mechanical properties of the thermoplastic resin are deteriorated.
In view of this, the embodiments of the present application improve the dispersibility of the composite material by adding the nucleating agent to the composite material. It should be noted that not any nucleating agent can be used to improve the dispersibility of the carbon nanotubes in the thermoplastic resin in the embodiments of the present application. In some embodiments, the nucleating agent provided in the embodiments of the present application is selected from one or more of silicate, stearate, nano-montmorillonite, carbon powder, zinc powder, barium sulfate, mica powder, talc, zinc oxide, carbonate, phosphate, sodium benzoate, monocarboxylate, benzoate, aromatic phosphate, aromatic sulfonate, polyethylene glycol diglycidyl ether, glycidyl methacrylate copolymer, polyolefin, polytetrafluoroethylene, ethylene-acrylic acid copolymer salt, polypentylene glycol dibenzoate, triphenyl phosphate, phthalate, and amide ester. Under the condition, the nucleating agent can modify the surface of the carbon nano tube, destroy the molecular interfacial force between the carbon nano tubes, reduce the combination between the carbon nano tubes, effectively improve the dispersibility and compatibility of the carbon nano tubes in a matrix, and refine and homogenize the size of a crystal area so that the network structure of the carbon nano tubes in the matrix is more perfect, thereby obviously improving the electrical property of the composite material. On the basis, the carbon nano tubes are uniformly dispersed in the thermoplastic resin through coating of other auxiliary materials, such as a compatilizer, a coupling agent and the like, and a good conductive network structure is constructed. Furthermore, in the system, the nucleating agent can provide required crystal nuclei in the crystallization process of a polymer matrix, namely thermoplastic resin, while dispersing the carbon nanotubes, so that the original homogeneous nucleation of the polymer is converted into heterogeneous nucleation, thereby accelerating the crystallization speed, refining the crystal grain structure, being beneficial to improving the rigidity of the product, shortening the molding period, keeping the dimensional stability of the final product, improving the transparency, the rigidity, the modulus and the like. The carbon nano tube can also obviously improve the mechanical property of the thermoplastic resin on the premise of good dispersion, the nucleating agent and the carbon nano tube form a synergistic effect on the property of the composite material, the nucleating agent or the carbon nano tube is beneficial to improving the mechanical properties of the composite material, such as tensile strength, bending strength, notch impact strength and the like, and the effect of improving the comprehensive property by adding the two components is better than the effect of independently adding one component. Finally, the composite material with the uniformly dispersed carbon nanotube network has good conductivity and comprehensive mechanical properties. In addition, the thermoplastic resin-based conductive composite material is prepared from the carbon nanotubes and the nucleating agent in the thermoplastic resin, so that the problem of secondary agglomeration of the carbon nanotubes due to the fact that the resin is changed from a solid state to a molten state after being reheated during subsequent injection molding or extrusion molding processing and the single injection molding or extrusion screw cannot provide the same shearing force as the modified granulation double screw can be solved.
In some embodiments, the nucleating agent has a particle size of 1-10 μm. In the embodiment of the application, the carbon nano tube has a nano-scale tube diameter and a micron-scale length, and the nucleating agent with the particle size of 1-10 mu m can form pi-pi conjugate construction with the carbon nano tube, which is equivalent to the fact that the nucleating agent is wound on the wall surface of the carbon nano tube, so that the improvement of the dispersion uniformity of the carbon nano tube in the thermoplastic resin is facilitated, and the nucleating agent and the carbon nano tube play the synergistic effect. If the particle size of the nucleating agent is too large, it cannot assist the uniform dispersion of the carbon nanotubes in the resin, but adversely affects the impact strength of the thermoplastic resin.
In some embodiments, the nucleating agent has a particle size of less than or equal to 1.3 μm. In this case, the mesh number of the nucleating agent is greater than or equal to 10000 meshes, which facilitates the formation of non-covalent bond connection between the nucleating agent and the carbon nanotubes and provides a dispersing effect on the carbon nanotubes; meanwhile, the particle size range is favorable for forming a synergistic effect with the carbon nano tubes with similar sizes, and the crystallization and the grain structure refinement of the thermoplastic resin are accelerated, so that the electrical and mechanical properties of the composite material are comprehensively improved.
In the embodiment of the application, the nucleating agent is 0-5 parts by weight but not 0 part by weight based on 100 parts by weight of the composite material. Exemplary, the nucleating agent is 0.1 part, 0.2 part, 0.5 part, 1 part, 5 parts, 1.5 parts, 2 parts, 2.5 parts, 3 parts, 2.5 parts, 4 parts, 5 parts, and the like, but is not limited thereto.
Because the carbon nanotubes have better dispersibility under the action of the nucleating agent, the dispersibility can be effectively improved, and therefore, in some embodiments, the total weight of the thermoplastic resin and the carbon nanotubes is 80 to 98 percent based on 100 percent of the total weight of the thermoplastic resin-based conductive composite material. In some embodiments, the combined weight of the thermoplastic resin and the carbon nanotubes is 80% to 95%, and illustratively, the combined weight of the thermoplastic resin and the carbon nanotubes is 80%, 82%, 85%, 88%, 90%, 91%, 92%, 93%, 94%, 95%. In this case, the content of other auxiliary materials added to the composite material is small, and the content of the thermoplastic resin and the carbon nanotubes is appropriate, so that the performance of the thermoplastic resin can be better ensured. In some embodiments, the total weight of the thermoplastic resin and the carbon nanotubes is 90% to 95% based on 100% of the total weight of the thermoplastic resin-based conductive composite. In some embodiments, the total weight of the thermoplastic resin and the carbon nanotubes is 80% to 90% based on 100% of the total weight of the thermoplastic resin-based conductive composite.
In the embodiment of the application, the compatilizer is added into the thermoplastic resin-based composite material to improve the compatibility of the carbon nanotubes and the thermoplastic resin and promote the uniform dispersion between the carbon nanotubes and the thermoplastic resin, so that the carbon nanotubes can build a conductive network between the thermoplastic resin.
In some embodiments, the compatibilizer is selected from one or more of a maleic anhydride grafted polyolefin elastomer, an acrylate-glycidyl ester-ethylene copolymer, a methacrylate-styrene butadiene rubber-styrene copolymer, an ethylene-acrylate copolymer, an ethylene vinyl acetate copolymer, an acrylonitrile-butadiene-styrene copolymer, an acrylonitrile-ethylene-styrene copolymer, and a block copolymer comprising a polyester hard segment and a polyether soft segment. The compatilizer is beneficial to improving the uniform distribution of the carbon nanotubes in the thermoplastic resin.
In the embodiment of the application, the part of the compatilizer is 0-6 parts but not 0 part based on 100 parts of the total weight of the composite material. Exemplary parts of the compatibilizer are, but not limited to, 0.1 part, 0.2 part, 0.5 part, 1 part, 5 parts, 1.5 parts, 2 parts, 2.5 parts, 3 parts, 2.5 parts, 4 parts, 5 parts, 6 parts, and the like.
In the embodiment of the application, the carbon nanotubes around the thermoplastic resin are bonded to the thermoplastic resin by adding the coupling agent, so that the carbon nanotubes are connected with the thermoplastic resin, and the conductivity of the composite material is improved. In some embodiments, the coupling agent is one or more of silanes, titanates, aluminates, phosphates.
In the embodiment of the application, the part of the coupling agent is 0-2 parts but not 0 part based on 100 parts of the total weight of the composite material. Exemplary parts of the compatibilizer are, but not limited to, 0.1 part, 0.2 part, 0.5 part, 0.8 part, 1.0 part, 1.2 parts, 1.4 parts, 1.5 parts, 1.8 parts, 2.0 parts, and the like.
In the embodiment of the application, the antioxidant is added to improve the oxidation resistance of the composite material. In some embodiments, the antioxidant is selected from one or more of 1010, 1098, 1076, 3114, 168, 626, 627A, 9228.
In the embodiment of the application, the part of the antioxidant is 0.2-1 part but not 0 part based on 100 parts of the total weight of the composite material. Exemplary antioxidant is 0.2 parts, 0.3 parts, 0.4 parts, 0.5 parts, 0.6 parts, 0.7 parts, 0.8 parts, 0.9 parts, 1 part and the like, but is not limited thereto.
In the embodiment of the application, other auxiliary agents can be added according to the actual application requirement of the composite material. In some embodiments, the other additives are selected from one or more of conventional additives such as uv absorbers, colorants, lubricants, mold release agents, silicone oils, white mineral oils, and the like, but are not limited thereto.
In the embodiment of the application, the parts of other additives are 0.2-4 parts but not 0 part based on 100 parts of the total weight of the composite material. Exemplary, the parts of the other additives are specific parts such as 0.2 part, 0.5 part, 0.8 part, 1.0 part, 1.5 part, 2.0 part, 2.5 parts, 3.0 part, 3.5 parts, 4.0 part, etc., but are not limited thereto.
The thermoplastic resin-based conductive composite material provided by the first aspect of the application examples can be prepared by the following method.
In a second aspect, embodiments of the present application provide a method for preparing a thermoplastic resin-based conductive composite material, including the following steps:
s01, weighing the raw material components according to the ligand of the thermoplastic resin-based conductive composite material in the first aspect;
s02, drying the thermoplastic resin-based conductive composite material at the temperature of 80-140 ℃ for 0-4 hours;
s03, adding the dried thermoplastic resin, the compatilizer, the nucleating agent, the antioxidant, other auxiliaries and the coupling agent into a stirrer respectively, and stirring and mixing for 3-5 minutes at the rotating speed of 200-500 rpm to obtain a uniformly mixed premix;
s04, adding carbon nanotubes into the premix, and stirring and mixing for 3-5 minutes at a rotating speed of 200-500 rpm to obtain a mixture;
and S05, adding the mixture into a double-screw extruder, and performing melt extrusion granulation, water cooling, air drying, grain cutting and drying to obtain the thermoplastic resin-based conductive composite material.
According to the preparation method of the thermoplastic resin-based conductive composite material, the thermoplastic resin is subjected to preheating treatment, the moisture of the thermoplastic resin is removed, the bonding force of a premix obtained by mixing the thermoplastic resin and the components except the carbon nano tubes is weakened, the carbon nano tubes can be endowed with good dispersibility in the step of adding the carbon nano tubes, the carbon nano tubes are uniformly dispersed in the thermoplastic resin with the help of the nucleating agent and other auxiliary components, and the good mechanical property and the low volume resistivity are realized.
In the above step S01, the formulation of the thermoplastic resin-based composite material, and the preferred case thereof, as described above, will not be described herein again for the sake of brevity.
In step S02, since water may affect the dispersion of the carbon nanotubes, in the embodiment of the present application, the water in the thermoplastic resin is removed by a heating process before the thermoplastic resin is mixed with other materials. Specifically, the drying is carried out for 0 to 4 hours at the temperature of 80 to 140 ℃. In some embodiments, the drying may be by means of a forced air drying or a desiccant dryer.
In the step S03, the dried thermoplastic resin, the compatibilizer, the nucleating agent, the antioxidant, the other additives, and the coupling agent are respectively added to a mixer, and are uniformly mixed by stirring. In some embodiments, the dried thermoplastic resin, the compatibilizer, the nucleating agent, the antioxidant, the other additives and the coupling agent are sequentially added into a stirrer and stirred. Wherein the stirring treatment is carried out at a rotation speed of 200-500 rpm for 3-5 minutes.
In the step S04, the premixing process is performed first, and the carbon nanotubes are added after the premixing process, so as to improve the dispersion uniformity of the carbon nanotubes in the premix. In some embodiments, carbon nanotubes are added to the premix, stirred and mixed at a rotation speed of 200 to 500 rpm for 3 to 5 minutes, the carbon nanotubes are dispersed with each other under the action of a nucleating agent, and the carbon nanotubes dispersed with each other are uniformly dispersed among thermoplastic resins under the action of a compatilizer and a coupling agent, so that a good conductive network structure is constructed.
In the step S05, the mixture is added into a twin-screw extruder, and the thermoplastic resin-based conductive composite material is obtained through melt extrusion granulation, water cooling, air drying, grain cutting and drying. The processing temperature of the twin-screw extruder is determined according to the melting temperature of various thermoplastic resin substrates, and in some embodiments, the step of adding the mixture to the twin-screw extruder is performed at a screw rotation speed of 400 to 900 rpm.
The following description will be given with reference to specific examples.
Examples 1 to 4 and comparative examples 1 to 3
A thermoplastic resin-based composite material having the formulation shown in Table 1 below. The preparation method of the thermoplastic resin matrix composite material comprises the following steps:
drying the raw material PC resin for 4 hours at the temperature of 110 ℃;
respectively adding the dried thermoplastic resin, the compatilizer, the nucleating agent, the antioxidant, other auxiliaries and the coupling agent into a stirrer, and stirring and mixing for 3-5 minutes at the rotating speed of 200-500 rpm to obtain a uniformly mixed premix; adding carbon nanotubes into the premix, and stirring and mixing for 3-5 minutes at a rotating speed of 200-500 rpm to obtain a mixture;
adding the mixture into a double-screw extruder, and performing melt extrusion granulation, water cooling, air drying, grain cutting and drying to obtain the thermoplastic resin-based conductive composite material; wherein, the processing technological conditions of the double-screw extruder are as follows:
1) the twin-screw extrusion temperature is as follows: a first area: 230 to 250 ℃; and a second zone: 270-290 ℃; and (3) three zones: 280-300 ℃; and (4) four areas: 280-300 ℃; and a fifth zone: 270-290 ℃; a sixth zone: 270-290 ℃; seven areas: 260-280 ℃; and eight regions: 250-270 ℃; nine areas: 250-270 ℃; ten areas: 240-260 ℃; a machine head: 280-300 ℃;
2) the rotation speed of the twin screw was 800 rpm.
TABLE 1
The thermoplastic resin-based composite materials provided in examples 1 to 4 and comparative examples 1 to 3 were subjected to performance tests, and the test standards and test results are shown in Table 2 below.
TABLE 2
As can be seen from table 2 above, compared with comparative example 2, the thermoplastic resin-based composite materials obtained in examples 1 to 4 of the present application, due to the addition of the nucleating agent, have balanced mechanical properties, excellent processability, low volume resistivity, and wide applicability. This is due to: under the synergistic action of the nucleating agent, the compatilizer and the coupling agent and the combined action of the high-speed twin-screw extrusion conditions, the problem of agglomeration and dispersion of the carbon nano tubes is solved, and the dispersed carbon nano tubes form a net-shaped communicated structure in the composite material, so that the conductive/antistatic thermoplastic resin matrix composite material is prepared.
The thermoplastic resin-based composite materials provided in comparative examples 1 and 3, although added with a nucleating agent, do not contain a compatibilizer, or do not contain a compatibilizer and a coupling agent, and the mechanical properties and the volume resistivity of the obtained composite materials cannot be compatible. This is due to: the carbon nanotubes dispersed by the nucleating agent are poor in dispersibility in the thermoplastic resin due to the lack of the effect of the coupling agent and the compatibilizing agent.
Examples 5 to 8, comparative examples 4 to 6
A thermoplastic resin-based composite material having the formulation shown in Table 3 below. The preparation method of the thermoplastic resin matrix composite material comprises the following steps:
drying a raw material HIPS resin for 2 hours at the temperature of 85 ℃;
respectively adding the dried thermoplastic resin, the compatilizer, the nucleating agent, the antioxidant, other auxiliaries and the coupling agent into a stirrer, and stirring and mixing for 3-5 minutes at the rotating speed of 200-500 rpm to obtain a uniformly mixed premix; adding carbon nanotubes into the premix, and stirring and mixing for 3-5 minutes at a rotating speed of 200-500 rpm to obtain a mixture;
adding the mixture into a double-screw extruder, and performing melt extrusion granulation, water cooling, air drying, grain cutting and drying to obtain the thermoplastic resin-based conductive composite material; wherein, the processing technological conditions of the double-screw extruder are as follows:
1) the twin-screw extrusion temperature is as follows: a first area: 150-170 ℃; and a second zone: 200-220 ℃; and (3) three zones: 210-230 ℃; and (4) four areas: 210-230 ℃; and a fifth zone: 200-220 ℃; a sixth zone: 180-200 ℃; seven areas: 180-200 ℃; and eight regions: 170-190 ℃; nine areas: 170-190 ℃; ten areas: 170-190 ℃; a machine head: 200-230 ℃;
2) the rotation speed of the twin screw was 800 rpm.
TABLE 3
The thermoplastic resin-based composite materials provided in examples 5 to 8 and comparative examples 4 to 6 were subjected to the performance test, and the test standards and test results are shown in Table 4 below.
TABLE 4
As can be seen from Table 4 above, compared with comparative example 5, the thermoplastic resin matrix composite materials obtained by examples 5-8 of the present application, due to the addition of the nucleating agent, have balanced mechanical properties, excellent processability, lower volume resistivity and wide applicability. This is due to: under the synergistic action of the nucleating agent, the compatilizer and the coupling agent and the combined action of the high-speed twin-screw extrusion conditions, the problem of agglomeration and dispersion of the carbon nano tubes is solved, and the dispersed carbon nano tubes form a net-shaped communicated structure in the composite material, so that the conductive/antistatic thermoplastic resin matrix composite material is prepared.
Comparative examples 4 and 6 provide thermoplastic resin-based composites that, despite the addition of a nucleating agent, do not contain a compatibilizing agent, or do not contain a compatibilizing agent and a coupling agent, and the mechanical properties and volume resistivity of the resulting composites are compromised. This is due to: the carbon nanotubes dispersed by the nucleating agent are poor in dispersibility in the thermoplastic resin due to the lack of the effect of the coupling agent and the compatibilizing agent.
Examples 9 to 12 and comparative examples 7 to 9
A thermoplastic resin-based composite material having the formulation shown in Table 5 below. The preparation method of the thermoplastic resin matrix composite material comprises the following steps:
drying raw materials of PPO resin and HIPS resin for 2 hours at the temperature of 85 ℃;
respectively adding the dried thermoplastic resin, the compatilizer, the nucleating agent, the antioxidant, other auxiliaries and the coupling agent into a stirrer, and stirring and mixing for 3-5 minutes at the rotating speed of 200-500 rpm to obtain a uniformly mixed premix; adding carbon nanotubes into the premix, and stirring and mixing for 3-5 minutes at a rotating speed of 200-500 rpm to obtain a mixture;
adding the mixture into a double-screw extruder, and performing melt extrusion granulation, water cooling, air drying, grain cutting and drying to obtain the thermoplastic resin-based conductive composite material; wherein, the processing technological conditions of the double-screw extruder are as follows:
1) the twin-screw extrusion temperature is as follows: a first area: 180-220 ℃; and a second zone: 250 to 280 ℃; and (3) three zones: 260-300 ℃; and (4) four areas: 260-300 ℃; and a fifth zone: 270-300 ℃; a sixth zone: 250 to 280 ℃; seven areas: 240-270 ℃; and eight regions: 230-260 ℃; nine areas: 220-250 ℃; ten areas: 220-250 ℃; a machine head: 260-300 ℃;
2) the rotation speed of the twin screw was 800 rpm.
TABLE 5
The thermoplastic resin-based composite materials provided in examples 9 to 12 and comparative examples 7 to 9 were subjected to the performance test, and the test standards and test results are shown in Table 6 below.
TABLE 6
As can be seen from Table 6, compared with comparative example 8, the thermoplastic resin matrix composite materials obtained by examples 9-12 of the present application, which are added with the nucleating agent, have balanced mechanical properties, excellent processability, lower volume resistivity and wide applicability. This is due to: under the synergistic action of the nucleating agent, the compatilizer and the coupling agent and the combined action of the high-speed twin-screw extrusion conditions, the problem of agglomeration and dispersion of the carbon nano tubes is solved, and the dispersed carbon nano tubes form a net-shaped communicated structure in the composite material, so that the conductive/antistatic thermoplastic resin matrix composite material is prepared.
Comparative examples 7 and 9 provide thermoplastic resin-based composites which, despite the addition of a nucleating agent, do not contain a compatibilizing agent, or do not contain a compatibilizing agent and a coupling agent, and which have a mechanical property and a volume resistivity that are not compatible. This is due to: the carbon nanotubes dispersed by the nucleating agent are poor in dispersibility in the thermoplastic resin due to the lack of the effect of the coupling agent and the compatibilizing agent.
In conclusion, the carbon nanotube/hot-melt resin-based conductive composite material prepared by the embodiment of the application has lower volume resistivity, and excellent impact resistance and tensile bending property.
The above description is only exemplary of the present application and should not be taken as limiting the present application, as any modification, equivalent replacement, or improvement made within the spirit and principle of the present application should be included in the protection scope of the present application.
Claims (10)
1. The thermoplastic resin-based conductive composite material is characterized by comprising the following components in parts by weight:
wherein the content of the compatilizer, the nucleating agent and the coupling agent is not 0.
2. The thermoplastic resin-based conductive composite material as claimed in claim 1, wherein the nucleating agent is selected from one or more of silicate, stearate, nano-montmorillonite, carbon powder, zinc powder, barium sulfate, mica powder, talc, zinc oxide, carbonate, phosphate, sodium benzoate, monocarboxylate, benzoate, aromatic phosphate, aromatic sulfonate, polyethylene glycol diglycidyl ether, glycidyl methacrylate copolymer, polyolefin, polytetrafluoroethylene, ethylene-acrylic acid copolymer salt, polypentylene glycol dibenzoate, triphenyl phosphate, phthalate, and amide ester.
3. The thermoplastic resin-based conductive composite material as claimed in claim 2, wherein the grain size of the nucleating agent is 1 to 10 μm.
4. The thermoplastic resin-based conductive composite material according to claim 1, wherein the total weight of the thermoplastic resin and the carbon nanotubes is 80 to 95% based on 100% of the total weight of the thermoplastic resin-based conductive composite material.
5. The thermoplastic resin based conductive composite material AS claimed in any of claims 1 to 4, characterized in that the thermoplastic resin is selected from one or several of PP, PE, AS, ABS, PS, PC, nylons, polyesters, PPO, PPS, POM, POK, LCP, HIPS.
6. The thermoplastic resin based conductive composite material according to any of claims 1 to 4, wherein the compatibilizer is selected from one or more of maleic anhydride grafted polyolefin elastomer, acrylate-glycidyl ester-ethylene copolymer, methacrylate-styrene butadiene rubber-styrene copolymer, ethylene-acrylate copolymer, ethylene vinyl acetate copolymer, acrylonitrile-butadiene-styrene copolymer, acrylonitrile-ethylene-styrene copolymer, block copolymer containing polyester hard segment and polyether soft segment.
7. The conductive composite material based on thermoplastic resin according to any of claims 1 to 4, characterized in that the coupling agent is one or more of silanes, titanates, aluminates, phosphates.
8. The thermoplastic resin based conductive composite material according to any of the claims 1 to 4, characterized in that the antioxidant is selected from one or several of 1010, 1098, 1076, 3114, 168, 626, 627A, 9228; and/or
The other auxiliary agents are selected from one or more of conventional additives such as ultraviolet absorbers, coloring agents, lubricants, mold release agents, silicone oil, white mineral oil and the like.
9. The preparation method of the thermoplastic resin-based conductive composite material is characterized by comprising the following steps of:
the ligand of the thermoplastic resin-based conductive composite material as defined in any one of claims 1 to 8, wherein the raw material components are weighed;
drying the thermoplastic resin-based conductive composite material for 0-4 hours at the temperature of 80-140 ℃;
respectively adding the dried thermoplastic resin, the compatilizer, the nucleating agent, the antioxidant, other auxiliaries and the coupling agent into a stirrer, and stirring and mixing for 3-5 minutes at the rotating speed of 200-500 rpm to obtain a uniformly mixed premix;
adding carbon nanotubes into the premix, and stirring and mixing for 3-5 minutes at a rotating speed of 200-500 rpm to obtain a mixture;
and adding the mixture into a double-screw extruder, and performing melt extrusion granulation, water cooling, air drying, grain cutting and drying to obtain the thermoplastic resin-based conductive composite material.
10. The method for preparing the thermoplastic resin-based conductive composite material as claimed in claim 9, wherein in the step of adding the mixture into a twin-screw extruder, the screw rotation speed is 400-900 rpm.
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Application publication date: 20210528 |