CN116003985B - Conductive glass fiber reinforced polycarbonate composite material and preparation method and application thereof - Google Patents
Conductive glass fiber reinforced polycarbonate composite material and preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to a glass fiber reinforced polycarbonate composite material with a conductive effect, and a preparation method and application thereof, and belongs to the technical field of high polymer materials. The composite material comprises the following components: PC:74.5 to 85.4 parts; carbon nanotubes: 4.0 to 6.0 parts; 1076:0.1 to 0.5 part; 168:0.1 to 0.5 part; PETS:0.1 to 2.0 parts; dimethicone: 0.1 to 0.5 part; hyper C100:0.2 to 2.0 parts; TCR442A:10.0 parts; the raw materials except the glass fiber are evenly mixed according to a specific process, and then are subjected to melt extrusion by a double-screw extruder through a main feed and a side feed together with the glass fiber, cooled by a cooling water tank and dehydrated by an air knife, and then cut into cylindrical granular materials with the thickness of 3-4 mm and the length of 3mm by a granulator. Meets the requirements of materials with high conductivity and physical properties in special fields.
Description
Technical Field
The invention relates to a glass fiber reinforced polycarbonate composite material with a conductive effect, and a preparation method and application thereof, and belongs to the technical field of high polymer materials.
Background
The product of the general glass fiber reinforced polycarbonate material is easy to generate static electricity in daily use, especially in a dry environment, if the static electricity accumulated on the surface of a plastic product cannot be released in time, the accumulated static electricity can be released when contacting, electric shock and damage to electronic components can be caused, so that instrument and equipment are failed, even the formed spark can cause explosion or fire, especially in special places such as gas stations and gas stations, which are easy to generate fire, and the damage of the static electricity is more serious. In a word, the damage caused by static electricity generated on the surface of the workpiece seriously affects life, production and daily work, and even sometimes causes serious accidents such as fire and explosion. The product injection-molded by the conductive glass fiber reinforced polycarbonate material can also shield electromagnetic waves, effectively protect electronic components in the product from the interference of external electromagnetic waves, and has more stable work.
The patent of the conductive glass fiber reinforced polycarbonate material has been filed, publication (bulletin) no: CN 104629284A A glass fiber reinforced antistatic Polycarbonate (PC) is prepared from nonionic antistatic agent with surface resistivity reaching antistatic level and conductivity not reaching level (surface resistance value not higher than 1×10) 5 Ω). Publication (bulletin) number: CN 103342884A high-performance antistatic glass fiber reinforced polycarbonate composite material, preparation method and application thereof, wherein the antistatic agent is an antistatic agent compounded by quaternary ammonium salt cationic surfactant and triethanolamine, and the surface resistance value is as low as 1 multiplied by 10 6 Ω is still higher than the conductivity level and some of its physical properties are reduced.
Disclosure of Invention
The invention solves the technical problems that: the conductive glass fiber reinforced polycarbonate composite material is provided, and has various physical properties superior to those of the common glass fiber reinforced polycarbonate composite material, so that the problems caused by static electricity generated and accumulated in the use process of a part injection molded by using glass fiber reinforced polycarbonate are solved, the cleanliness, the accuracy and the safety of an electric appliance in use are ensured, and the strength and the melt index of the polycarbonate material are improved.
In order to solve the technical problems, the technical scheme provided by the invention is as follows: the conductive glass fiber reinforced polycarbonate composite material comprises the following components in parts by weight:
polycarbonate PC:74.5 to 85.4 parts;
carbon nanotubes: 4.0 to 6.0 parts;
hindered phenolic antioxidant 1076:0.1 to 0.5 part;
phosphite antioxidant 168:0.1 to 0.5 part;
lubricant PETS:0.1 to 2.0 parts;
dimethicone: 0.1 to 0.5 part;
flow aid Hyper C100:0.2 to 2.0 parts;
glass fiber TCR442A:10.0 parts;
the density of the polycarbonate PC is 1.18-1.22, the glass transition temperature is 145-150 ℃, and the corresponding thermal deformation temperature is 130-140 ℃;
the flow aid is resin with density of 1.10g/cm < 3 >, melting range of 140-180 ℃ and hyperbranched structure, and commercial brand is Hyper C100;
the glass fiber TCR442A is alkali-free chopped glass fiber, has the fiber diameter of 11-17 mu m and the fiber length of 3.0-4.5mm, is subjected to surface treatment by a coupling agent, and is suitable for a polycarbonate system.
Preferably, the composition comprises the following components in parts by weight:
polycarbonate PC:81 parts;
carbon nanotubes: 6.0 parts;
hindered phenolic antioxidant 1076:0.1 part;
phosphite antioxidant 168:0.2 parts;
lubricant PETS:0.2 parts;
dimethicone: 0.5 parts;
flow aid Hyper C100:2 parts;
glass fiber TCR442A:10.0 parts.
In order to solve the technical problems, another technical scheme provided by the invention is as follows: the preparation method of the conductive glass fiber reinforced polycarbonate composite material comprises the following steps:
(1) Drying the polycarbonate at 120 ℃ for 2-4 hours, and controlling the moisture content in the polycarbonate to be below 0.1%;
(2) Adding 74.5 to 85.4 parts of polycarbonate into a stirring pot, stirring at a rotating speed of 100 to 200rpm, adding 0.1 to 0.5 part of simethicone, stirring for 2 to 3 minutes, uniformly attaching the simethicone on the surfaces of polycarbonate particles, adding 4 to 6 parts of carbon nano tube powder while stirring at a rotating speed of 100 to 200rpm, stirring at a rotating speed of 600 to 800rpm for 5 to 6 minutes, uniformly mixing, reducing the rotating speed to 100 to 200rpm, and stirring while adding 0.1 to 0.5 part of antioxidant 1076 and 0.1 to 0.5 part of phosphate antioxidant 168; adding 0.1-2 parts of PETS lubricant and 0.2-2.0 parts of flow aid Hyper C100 into a stirring pot, increasing the rotating speed to 200-300 rpm, continuously stirring for 2-3 minutes, and uniformly mixing to obtain a mixed material;
(3) The mixed material is added into a main feeding port of a double-screw extruder through a main feeding scale, chopped glass fiber TCR442A is added into the extruder through side feeding through a side feeding scale of the double-screw extruder, the barrel temperature of the double-screw extruder is controlled at 200-280 ℃, the screw rotating speed is 300-400 rpm, the mass ratio of glass fiber in the composite material is adjusted to 10% by adjusting the ratio of the blanking amount of the main feeding scale and the blanking amount of the side feeding scale of the double-screw extruder, and extruded sample bars are cut into cylindrical granular materials with the thickness of 3-4 mm and the length of 3mm by a granulator after being cooled by a water tank and dehydrated by an air knife.
(4) And (3) drying the prepared polycarbonate composite material at 120 ℃ for 2-4 hours, preparing standard sample bars by using an injection molding machine, and testing according to the standard.
Preferably, the method comprises the following steps:
(1) 81.0 parts of polycarbonate, 6.0 parts of carbon nano tube, 0.1 part of antioxidant 1076, 0.2 part of antioxidant 168, 0.2 part of PETS, 0.5 part of simethicone, 2.0 parts of Hyper C100 and 10.0 parts of glass fiber TCR442A are weighed;
(2) Adding 81.0 parts of polycarbonate in the step (1) into a stirring pot, stirring at a rotating speed of 120rpm, adding 0.5 part of dimethyl silicone oil, stirring for 3 minutes to uniformly attach a silicone oil dispersing agent to the surfaces of polycarbonate particles, adding 6.0 parts of carbon nano tube powder, stirring at a rotating speed of 120rpm, stirring at a rotating speed of 800rpm for 6 minutes, uniformly mixing, reducing the rotating speed to 120rpm, adding 0.1 part of hindered phenol antioxidant 1076, 0.2 part of phosphite antioxidant 168, 0.2 part of PETS lubricant and 2.0 parts of Hyper C100 into the stirring pot, continuously stirring for 3 minutes, and uniformly mixing to obtain a mixed material; the mixed material is added from a main feeding port of an extruder through a weight loss scale, 10.0 parts of glass fiber TCR442A is added from a side feeding port through the weight loss scale, and the conductive glass fiber reinforced polycarbonate composite material is obtained through extrusion granulation.
In order to solve the technical problems, another technical scheme provided by the invention is as follows: the conductive glass fiber reinforced polycarbonate composite material can be applied to parts which need to be shielded from electromagnetic waves or require antistatic.
The invention has the beneficial effects that:
the conductive glass fiber reinforced polycarbonate composite material has the advantages that all the components play a synergistic role, the physical properties of the conductive glass fiber reinforced polycarbonate composite material can reach the physical properties of the common glass fiber reinforced polycarbonate material, the conductive glass fiber reinforced polycarbonate material also has the electrical conductivity which the common glass fiber reinforced polycarbonate material does not have, and all other physical properties of the conductive glass fiber reinforced polycarbonate composite material are superior to those of the common glass fiber reinforced polycarbonate material, so that the conductive glass fiber reinforced polycarbonate composite material is suitable for parts which cannot generate static electricity, are conductive or need to shield external electromagnetic waves, and are required to have good fluidity and complex structures.
The material uses carbon nano tube as conductive auxiliary agent, and its addition quantity is small, so that its comprehensive cost is low. The polycarbonate resin with high melt index is selected as the raw material, and the flow additive Hyper C100 is added, so that the material has good fluidity, is easy to carry out injection molding processing, is suitable for injection molding of a product with a complex structure, and has good surface effect. The glass fiber is alkali-free chopped glass fiber with the monofilament diameter of 11-17 mu m, the high length-diameter ratio is maintained in the material, and the surface treated by the coupling agent ensures that the glass fiber is combined with the resin more firmly, thereby improving the physical property of the material.
The high-torque homodromous double-screw extruder is adopted, the motor power is high, the torque is high, the temperature control is accurate, and the driving force of the extruder and the stability of materials are ensured. The vacuumizing system can effectively suck away small molecular substances generated in the material or in the extrusion process, and ensures that the material does not contain small molecular impurities, so that the material has stable and higher physical properties.
In both comparative example 2 and comparative example 3, where no flow aid was added, the melt index was significantly lower than that of comparative example, indicating that the addition of carbon nanotubes significantly reduced the melt index of the glass fiber reinforced polycarbonate material, while it can also be seen that the conductivity of comparative example 2, where the addition of dimethicone was superior to that of comparative example 3, where no dimethicone was added, indicating that the addition of dimethicone and the special compounding process increased the conductivity of carbon nanotubes in the glass fiber reinforced polycarbonate material.
The tensile strength of examples 1-4 and comparative examples 1-3 was about 2-7 MPa higher than that of comparative example 4, indicating that the addition of carbon nanotubes improved the strength of the conventional glass fiber reinforced polycarbonate material, the notched Izod impact strength of examples 1-4 was substantially the same as that of comparative example 4, and the surface resistance values of examples 1-4 and comparative examples 1-3 were much lower than that of comparative example 4, 10 14 Omega, has better conductive effect, meets the requirements of material conduction and shielding of external electromagnetic waves in specific fields.
The tensile strength of example 4 is 4MPa higher than that of comparative example 1, indicating that the glass fiber content has a positive effect on the strength of the polycarbonate composite, but that a high glass fiber content reduces the melt index of the polycarbonate composite, resulting in the appearance of a surface of the article with a defect of non-smooth floating fibers. Through a number of experiments conducted by the inventors, it was unexpectedly obtained that example 4 is a conductive glass fiber reinforced polycarbonate composite material that is the best formulation, and that the components exert a synergistic effect. From the physical properties and surface resistances of examples 1 to 4 and comparative examples 1 to 4, it can be seen that: the tensile strength of example 4 is highest, the surface resistance is lowest, i.e., the conductivity is best, the notched Izod impact strength is equal to other examples and comparative examples, the melt index is higher, and the formulation is best. The innovative compounding process of example 4 is also an indispensable process step for the optimal formulation system.
In summary, through the innovative compounding of the raw materials, the dispersing agent and the flow aid to improve the conductive effect and the melt index, the innovative design of the mixing process and the optimization of the extrusion process, the conductive glass fiber reinforced polycarbonate material is produced, and the special requirements of the complex components with high melt index and high structure in the specific field are met.
Detailed Description
Example 1
(1) The conductive glass fiber reinforced polycarbonate material comprises the following components in parts by weight:
84.0 parts of polycarbonate (Wanhua chemistry, trade mark A1220), 4.0 parts of carbon nanotubes (Qingdao Chaorei, trade mark CR 5102), 0.1 parts 1076, 0.2 parts 168, 0.2 parts PETS, 0.5 parts simethicone, 1.0 part HyperC 100, 10.0 parts glass fiber TCR442A;
the density of the polycarbonate PC is 1.18-1.22, the glass transition temperature is 145-150 ℃, and the corresponding thermal deformation temperature is 130-140 ℃;
the flow aid has a density of 1.10g/cm 3 The melting range is 140-180 ℃ resin with a hyperbranched structure, and the commercial brand is Hyper C100;
the glass fiber TCR442A is alkali-free chopped glass fiber with the diameter of 11-17 mu m and the length of 3.0-4.5mm, and is subjected to surface treatment by a coupling agent; is suitable for polycarbonate systems.
(2) Adding 84.0 parts of polycarbonate in the step (1) into a stirring pot, stirring at a rotating speed of 120rpm, adding 0.5 part of dimethyl silicone oil, stirring for 3 minutes, uniformly attaching a silicone oil dispersing agent to the surfaces of polycarbonate particles, adding 4.0 parts of carbon nano tube powder, stirring at a rotating speed of 120rpm, stirring for 6 minutes, uniformly mixing, reducing the rotating speed to 120rpm, adding 0.1 part of hindered phenol antioxidant 1076, 0.2 part of phosphite antioxidant 168, 0.2 part of PETS lubricant and 1.0 part of Hyper C100 into the stirring pot, continuously stirring for 3 minutes, and uniformly mixing to obtain a mixed material. The mixture was fed from the main feeding port of the extruder through a weight loss scale, 10.0 parts of glass fiber TCR442A was fed from the side feeding port through a weight loss scale, and extrusion granulation was performed according to the process parameters of Table 1, to obtain a polycarbonate composite material of example 1.
Table 1: extruder production process parameter setting table
Example 2
(1) 83.0 parts of polycarbonate (Wanhua chemistry, trade mark A1220), 5.0 parts of carbon nanotubes (Qingdao Chaorei, trade mark CR 5102), 0.1 parts 1076, 0.2 parts 168, 0.2 parts PETS, 0.5 parts simethicone, 1.0 part HyperC 100, 10.0 parts glass fiber TCR442A are weighed;
(2) Adding 83.0 parts of polycarbonate in the step (1) into a stirring pot, stirring at a rotating speed of 120rpm, adding 0.5 part of dimethyl silicone oil, stirring for 3 minutes, uniformly attaching a silicone oil dispersing agent to the surfaces of polycarbonate particles, adding 5.0 parts of carbon nano tube powder, stirring at a rotating speed of 120rpm, stirring for 6 minutes, uniformly mixing, reducing the rotating speed to 120rpm, adding 0.1 part of hindered phenol antioxidant 1076, 0.2 part of phosphite antioxidant 168, 0.2 part of PETS lubricant and 1.0 part of Hyper C100 into the stirring pot, continuously stirring for 3 minutes, and uniformly mixing to obtain a mixed material. The mixture was fed from the main feeding port of the extruder through a weight loss scale, 10.0 parts of glass fiber TCR442A was fed from the side feeding port through a weight loss scale, and extrusion granulation was performed according to the process parameters of Table 1, to obtain a polycarbonate composite material of example 2.
Example 3
(1) 82.0 parts of polycarbonate (Wanhua chemistry, trade mark A1220), 6.0 parts of carbon nanotubes (Qingdao Chaorei, trade mark CR 5102), 0.1 parts 1076, 0.2 parts 168, 0.2 parts PETS, 0.5 parts simethicone, 1.0 part HyperC 100, 10.0 parts glass fiber TCR442A are weighed;
(2) Adding 82.0 parts of polycarbonate in the step (1) into a stirring pot, stirring at a rotating speed of 120rpm, adding 0.5 part of dimethyl silicone oil, stirring for 3 minutes, uniformly attaching a silicone oil dispersing agent to the surfaces of polycarbonate particles, adding 6.0 parts of carbon nano tube powder, stirring at a rotating speed of 120rpm, stirring for 6 minutes, uniformly mixing, reducing the rotating speed to 120rpm, adding 0.1 part of hindered phenol antioxidant 1076, 0.2 part of phosphite antioxidant 168, 0.2 part of PETS lubricant and 1.0 part of Hyper C100 into the stirring pot, continuously stirring for 3 minutes, and uniformly mixing to obtain a mixed material. The mixture was fed from the main feeding port of the extruder through a weight loss scale, 10.0 parts of glass fiber TCR442A was fed from the side feeding port through a weight loss scale, and extrusion granulation was performed according to the process parameters of Table 1, to obtain a polycarbonate composite material of example 3.
Example 4
(1) Drying the polycarbonate at 120 ℃ for 2-4 hours, and controlling the moisture content in the polycarbonate to be below 0.1%; 81.0 parts of polycarbonate (Wanhua chemical, trade mark A1220), 6.0 parts of carbon nanotubes (Qingdao Chaorei, trade mark CR 5102), 0.1 parts of antioxidant 1076, 0.2 parts of antioxidant 168, 0.2 parts of lubricant PETS, 0.5 parts of simethicone, 2.0 parts of flow aid HyperC 100, 10.0 parts of glass fiber TCR442A are weighed; the density of the polycarbonate PC is 1.18-1.22, the glass transition temperature is 145-150 ℃, and the corresponding thermal deformation temperature is 130-140 ℃; the flow aid is resin with density of 1.10g/cm < 3 >, melting range of 140-180 ℃ and hyperbranched structure, and commercial brand is Hyper C100; the glass fiber TCR442A is alkali-free chopped glass fiber with the diameter of 11-17 mu m and the length of 3.0-4.5mm.
(2) Adding 81.0 parts of polycarbonate in the step (1) into a stirring pot, stirring at a rotating speed of 120rpm, adding 0.5 part of dimethyl silicone oil, stirring for 3 minutes, uniformly attaching a silicone oil dispersing agent to the surfaces of polycarbonate particles, adding 6.0 parts of carbon nano tube powder, stirring at a rotating speed of 120rpm, stirring for 6 minutes, uniformly mixing, reducing the rotating speed to 120rpm, adding 0.1 part of hindered phenol antioxidant 1076, 0.2 part of phosphite antioxidant 168, 0.2 part of PETS lubricant and 2.0 parts of Hyper C100 into the stirring pot, continuously stirring for 3 minutes, and uniformly mixing to obtain a mixed material. The mixture was fed from the main feeding port of the extruder through a weight loss scale, 10.0 parts of glass fiber TCR442A was fed from the side feeding port through a weight loss scale, and extrusion granulation was performed according to the process parameters of Table 1, to obtain a polycarbonate composite material of example 4.
And (3) drying the prepared polycarbonate composite material at 120 ℃ for 2-4 hours, preparing standard sample bars by using an injection molding machine, and testing according to the standard.
Comparative example 1
(1) 83.0 parts of polycarbonate (Wanhua chemistry, trade mark A1220), 6.0 parts of carbon nanotubes (Qingdao Chaorei, trade mark CR 5102), 0.1 parts 1076, 0.2 parts 168, 0.2 parts PETS, 0.5 parts simethicone, 2.0 parts HyperC 100, 8.0 parts glass fiber TCR442A are weighed;
(2) Adding 83.0 parts of polycarbonate in the step (1) into a stirring pot, stirring at a rotating speed of 120rpm, adding 0.5 part of dimethyl silicone oil, stirring for 3 minutes, uniformly attaching a silicone oil dispersing agent to the surfaces of polycarbonate particles, adding 6.0 parts of carbon nano tube powder, stirring at a rotating speed of 120rpm, stirring for 6 minutes, uniformly mixing, reducing the rotating speed to 120rpm, adding 0.1 part of hindered phenol antioxidant 1076, 0.2 part of phosphite antioxidant 168, 0.2 part of PETS lubricant and 2.0 parts of Hyper C100 into the stirring pot, continuously stirring for 3 minutes, and uniformly mixing to obtain a mixed material. The mixture was fed from the main feeding port of the extruder through a weight loss scale, 8.0 parts of glass fiber TCR442A was fed from the side feeding port through a weight loss scale, and extrusion granulation was performed according to the process parameters of Table 1, to obtain a polycarbonate composite material of comparative example 1.
Comparative example 2
(1) 83.0 parts of polycarbonate (Wanhua chemical, trade mark A1220), 6.0 parts of carbon nanotubes (Qingdao Chaorei, trade mark CR 5102), 0.1 parts of 1076, 0.2 parts of 168, 0.2 parts of PETS, 0.5 parts of simethicone and 10.0 parts of glass fiber TCR442A are weighed;
(2) Adding 83.0 parts of polycarbonate in the step (1) into a stirring pot, stirring at a rotating speed of 120rpm, adding 0.5 part of dimethyl silicone oil, stirring for 3 minutes, uniformly attaching a silicone oil dispersing agent to the surfaces of polycarbonate particles, adding 6.0 parts of carbon nano tube powder, stirring at a rotating speed of 120rpm, stirring for 6 minutes, uniformly mixing, reducing the rotating speed to 120rpm, adding 0.1 part of hindered phenol antioxidant 1076, 0.2 part of phosphite antioxidant 168 and 0.2 part of PETS lubricant into the stirring pot, increasing the rotating speed to 200rpm, and continuously stirring for 3 minutes, uniformly mixing, thereby obtaining a mixed material. The mixture was fed from the main feeding port of the extruder through a weight loss scale, 10.0 parts of glass fiber TCR442A was fed from the side feeding port through a weight loss scale, and extrusion granulation was performed according to the process parameters of Table 1, to obtain a polycarbonate composite material of comparative example 2.
Comparative example 3
(1) 83.5 parts of polycarbonate (Wanhua chemistry, trade mark A1220), 6.0 parts of carbon nanotubes (Qingdao Chaorei, trade mark CR 5102), 0.1 parts 1076, 0.2 parts 168, 0.2 parts PETS, 10.0 parts glass fiber TCR442A are weighed;
(2) Adding 83.5 parts of polycarbonate in the step (1) into a stirring pot, stirring at a rotation speed of 120rpm, adding 6.0 parts of carbon nano tube powder, stirring at a rotation speed of 800rpm for 6 minutes, uniformly mixing, reducing the rotation speed to 120rpm, adding 0.1 part of hindered phenol antioxidant 1076, 0.2 part of phosphite antioxidant 168 and 0.2 part of PETS lubricant into the stirring pot while stirring, increasing the rotation speed to 200rpm, and continuously stirring for 3 minutes, uniformly mixing, thus obtaining a mixed material. The mixture was fed from the main feeding port of the extruder through a weight loss scale, 10.0 parts of glass fiber TCR442A was fed from the side feeding port through a weight loss scale, and extrusion granulation was performed according to the process parameters of Table 1, to obtain a polycarbonate composite material of comparative example 3.
Comparative example 4
(1) 89.5 parts of polycarbonate (Wanhua chemical, trade name A1220), 0.1 part 1076, 0.2 part 168, 0.2 part PETS, 10.0 parts glass fiber TCR442A are weighed out;
(2) Adding 89.5 parts of polycarbonate in the step (1) into a stirring pot, adding 0.1 part of hindered phenol antioxidant 1076, 0.2 part of phosphite antioxidant 168 and 0.2 part of PETS lubricant into the stirring pot while stirring at a rotating speed of 120rpm, increasing the rotating speed to 200rpm, and continuously stirring for 3 minutes to uniformly mix to obtain a mixed material. The mixture was fed from the main feeding port of the extruder through a weight loss scale, 10.0 parts of glass fiber TCR442A was fed from the side feeding port through a weight loss scale, and extrusion granulation was performed according to the process parameters of Table 1, to obtain a polycarbonate composite material of comparative example 4.
Comparative example 5
(1) 81.0 parts of polycarbonate (Wanhua chemical, trade mark A1220), 6.0 parts of carbon nanotubes (Qingdao Chaorei, trade mark CR 5102), 0.1 part of antioxidant 1076, 0.2 part of antioxidant 168, 0.2 part of lubricant PETS, 0.5 part of simethicone, 2.0 parts of annular flow aid and 10.0 parts of glass fiber TCR442A are weighed;
(2) Adding 81.0 parts of polycarbonate in the step (1) into a stirring pot, stirring at a rotating speed of 120rpm, adding 0.5 part of dimethyl silicone oil, stirring for 3 minutes, uniformly attaching a silicone oil dispersing agent to the surfaces of polycarbonate particles, adding 6.0 parts of carbon nano tube powder, stirring at a rotating speed of 120rpm, stirring for 6 minutes, uniformly mixing, reducing the rotating speed to 120rpm, adding 0.1 part of hindered phenol antioxidant 1076, 0.2 part of phosphite antioxidant 168, 0.2 part of PETS lubricant and 2.0 parts of annular flow aid into the stirring pot, increasing the rotating speed to 200rpm, and continuously stirring for 3 minutes, uniformly mixing, thereby obtaining a mixed material. The mixture was fed from the main feeding port of the extruder through a weight loss scale, 10.0 parts of glass fiber TCR442A was fed from the side feeding port through a weight loss scale, and extrusion granulation was performed according to the process parameters of Table 1, to obtain a polycarbonate composite material of comparative example 5.
The polycarbonate composite materials prepared in examples 1 to 4 and comparative examples 1 to 5 were dried at 120℃for 2 to 4 hours, then were manufactured into standard bars by an injection molding machine, and then tested according to the standard, and the test data are shown in Table 3. Glass fiber content was measured according to ISO 1172, melt index according to ISO 1133, tensile strength according to ISO 527, notched Izod impact strength according to ISO 180, surface resistance value according to EN 1149-1 standard.
Table 2: formulas of examples 1 to 4 and comparative examples 1 to 5
Table 3: physical properties and surface resistance of examples 1 to 4 and comparative examples 1 to 5
From the test data of physical properties and surface resistances of examples 1 to 4 and comparative examples 1 to 5 in Table 3, it can be seen that:
the melt index of examples 1 to 3 gradually decreased with the increase of the carbon nanotube addition amount, but the surface resistance gradually decreased, indicating that the conductivity gradually increased;
the melt index and tensile strength of example 4 are both higher than those of example 3, indicating that increasing the amount of flow aid Hyper C100 added increases the melt index and tensile strength of the composite;
in the comparison example 2 and the comparison example 3 without adding the flow aid, the melt indexes are both greatly lower than those of the comparison example, which shows that the addition of the carbon nano tube can greatly reduce the melt index of the glass fiber reinforced polycarbonate material, and meanwhile, the conductivity of the comparison example 2 with adding the dimethyl silicone oil is better than that of the comparison example 3 without adding the dimethyl silicone oil, which shows that the addition of the dimethyl silicone oil and the special mixing process can improve the conductivity of the carbon nano tube in the glass fiber reinforced polycarbonate material;
from example 4 and comparative example 1, it can be seen that the melt index of the composite material having a high glass fiber content is low, and that the glass fiber content of comparative example 5 is 0.2% lower than that of example 4, whereas the melt index of example 4 is higher than that of comparative example 5, indicating that the effect of the flow aid Hyper C100 having a "hyperbranched" structure on increasing the melt index of the glass fiber-reinforced polycarbonate material is superior to that of the annular flow aid, and that other data including surface resistance are substantially the same.
The tensile strength of examples 1-4 and comparative examples 1-3 was about 2-7 MPa higher than that of comparative example 4, indicating that the addition of carbon nanotubes improved the strength of the conventional glass fiber reinforced polycarbonate material, the notched Izod impact strength of examples 1-4 was substantially the same as that of comparative example 4, and the surface resistance values of examples 1-4 and comparative examples 1-3 were much lower than that of comparative example 4, 10 14 Omega has better conductive effect, and meets the requirement of material conduction in specific fields.
The tensile strength of example 4 is 4MPa higher than that of comparative example 1, indicating that the glass fiber content has a positive effect on the strength of the polycarbonate composite, but if the glass fiber content is too high, the melt index of the polycarbonate composite is lowered, and the surface of the article is subject to the defect of floating fiber smoothness.
From the physical properties and surface resistances of examples 1 to 4 and comparative examples 1 to 5, it can be seen that: the tensile strength of example 4 is highest, the surface resistance is lowest, i.e., the conductivity is best, the notched Izod impact strength is equal to other examples and comparative examples, the melt index is higher, and the formulation is best. The innovative compounding process of example 4 is also an indispensable process step for the optimal formulation system. In the prior art, all raw materials except glass fibers and containing antistatic agents are placed into a stirring pot for mixing at one time, and the invention adopts the process of step-by-step and sequential mixing in example 4 for mixing, so that carbon nanotubes can be effectively dispersed to improve conductivity and help auxiliary agents to be uniformly adhered to the surface of polycarbonate, and the effect of each auxiliary agent is greatly exerted.
The foregoing examples are provided for the purpose of illustration only, and are not intended to limit the scope of the invention, as the design considerations, alternatives to different raw materials and variations in number are within the scope of the invention.
Claims (5)
1. The conductive glass fiber reinforced polycarbonate composite material is characterized by comprising the following components in parts by weight:
polycarbonate PC:74.5 to 85.4 parts;
carbon nanotubes: 4.0 to 6.0 parts;
hindered phenolic antioxidant 1076:0.1 to 0.5 part;
phosphite antioxidant 168:0.1 to 0.5 part;
lubricant PETS:0.1 to 2.0 parts;
dimethicone: 0.1 to 0.5 part;
flow aid Hyper C100:0.2 to 2.0 parts;
glass fiber TCR442A:10.0 parts;
the density of the polycarbonate PC is 1.18-1.22, the glass transition temperature is 145-150 ℃, and the corresponding thermal deformation temperature is 130-140 ℃;
the flow aid has a density of 1.10g/cm 3 The melting range is 140-180 ℃ resin with a hyperbranched structure, and the commercial brand is Hyper C100;
the glass fiber TCR442A is alkali-free chopped glass fiber, the fiber diameter is 11 mu m-17 mu m, and the length is 3.0-4.5mm.
2. The conductive glass fiber reinforced polycarbonate composite material of claim 1, which is composed of the following components in parts by weight:
polycarbonate PC:81 parts;
carbon nanotubes: 6.0 parts;
hindered phenolic antioxidant 1076:0.1 part;
phosphite antioxidant 168:0.2 parts;
lubricant PETS:0.2 parts;
dimethicone: 0.5 parts;
flow aid Hyper C100:2 parts;
glass fiber TCR442A:10.0 parts.
3. The method for preparing the conductive glass fiber reinforced polycarbonate composite material according to claim 1, wherein the method comprises the following steps: comprises the following steps:
(1) Drying the polycarbonate at 120 ℃ for 2-4 hours, and controlling the moisture content in the polycarbonate to be below 0.1%;
(2) Adding 74.5 to 85.4 parts of polycarbonate into a stirring pot, stirring at a rotating speed of 100 to 200rpm, adding 0.1 to 0.5 part of simethicone, stirring for 2 to 3 minutes, uniformly attaching the simethicone on the surfaces of polycarbonate particles, adding 4 to 6 parts of carbon nano tube powder while stirring at a rotating speed of 100 to 200rpm, stirring at a rotating speed of 600 to 800rpm for 5 to 6 minutes, uniformly mixing, reducing the rotating speed to 100 to 200rpm, and stirring while adding 0.1 to 0.5 part of antioxidant 1076 and 0.1 to 0.5 part of phosphate antioxidant 168; adding 0.1-2 parts of PETS lubricant and 0.2-2.0 parts of flow aid Hyper C100 into a stirring pot, increasing the rotating speed to 200-300 rpm, continuously stirring for 2-3 minutes, and uniformly mixing to obtain a mixed material;
(3) The mixed material is added into a main feeding port of a double-screw extruder through a main feeding scale, chopped glass fiber TCR442A is added into the extruder through a side feeding port through a side feeding scale of the double-screw extruder, the barrel temperature of the double-screw extruder is controlled at 200-280 ℃, the screw rotating speed is 300-400 rpm, the proportion of the blanking amount of the main feeding scale of the double-screw extruder to the blanking amount of the side feeding scale is regulated, the mass ratio of glass fiber in the composite material is 10%, and extruded sample bars are cut into cylindrical granular materials with the thickness of 3-4 mm and the length of 3mm by a granulator after being cooled by a water tank and dehydrated by an air knife.
4. The method for preparing a conductive glass fiber reinforced polycarbonate composite material according to claim 3, wherein: comprises the following steps:
(1) 81.0 parts of polycarbonate, 6.0 parts of carbon nano tube, 0.1 part of antioxidant 1076, 0.2 part of antioxidant 168, 0.2 part of PETS, 0.5 part of simethicone, 2.0 parts of Hyper C100 and 10.0 parts of glass fiber TCR442A are weighed;
(2) Adding 81.0 parts of polycarbonate in the step (1) into a stirring pot, stirring at a rotating speed of 120rpm, adding 0.5 part of dimethyl silicone oil, stirring for 3 minutes to uniformly attach a silicone oil dispersing agent to the surfaces of polycarbonate particles, adding 6.0 parts of carbon nano tube powder, stirring at a rotating speed of 120rpm, stirring at a rotating speed of 800rpm for 6 minutes, uniformly mixing, reducing the rotating speed to 120rpm, adding 0.1 part of hindered phenol antioxidant 1076, 0.2 part of phosphite antioxidant 168, 0.2 part of PETS lubricant and 2.0 parts of Hyper C100 into the stirring pot, continuously stirring for 3 minutes, and uniformly mixing to obtain a mixed material; the mixed material is added from a main feeding port of an extruder through a main feeding scale, 10.0 parts of glass fiber TCR442A is added from a side feeding port through a side feeding scale, and the conductive glass fiber reinforced polycarbonate composite material is obtained through extrusion granulation.
5. Use of a conductive glass fiber reinforced polycarbonate composite according to claim 1 or 2, characterized in that: can be applied to the parts which need to shield electromagnetic waves or require antistatic.
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