CN114974684A - Wear-resistant tear-resistant silicone rubber wire cable and preparation method thereof - Google Patents
Wear-resistant tear-resistant silicone rubber wire cable and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a wear-resistant tear-resistant silicone rubber wire and cable and a preparation method thereof, and relates to the technical field of wire and cable production. The wear-resistant tear-resistant silicone rubber wire and cable prepared by the invention comprises a conductor, an insulating layer, a shielding layer and a sheath layer; wherein the insulating layer and the sheath layer are made of ceramic silicon rubber, and the shielding layer is made of polyamide aerogel; the self-made glass powder comprises calcium carbonate, zinc oxide, boric acid, ammonium dihydrogen phosphate and ammonium polyphosphate microspheres, not only enhances the flame retardance, but also has higher density and strength after being made into porcelain, and enhances the strength of the wire and cable after being made into porcelain; the polyamide aerogel introduces melamine into a polyamide main chain, and modified multi-walled carbon nanotubes are added to enhance the tear resistance and the shielding performance.
Description
Technical Field
The invention relates to the technical field of wire and cable production, in particular to a wear-resistant tear-resistant silicone rubber wire and cable and a preparation method thereof.
Background
Although the mineral insulation fireproof cable has good fire resistance, the manufacturing process is complex, the production cost is high, the manufacturing length is limited, the cable is very hard and cannot be bent, the joint is complex, the construction difficulty is high, and the cable is difficult to be widely applied. Although the mica tape wrapped fire-resistant cable is simple in process and unlimited in manufacturing length, the mica tape generally has a defect that the mechanical strength of the mica tape is greatly reduced after high-temperature combustion, the mica tape becomes brittle and is easy to pulverize and fall off after being subjected to severe vibration, and the fire-resistant effect is poor. And the mica tape is easy to fall off when being rubbed, so that a large amount of dust on a wrapping site threatens the health of operating personnel.
In recent years, researchers have explored and researched the ceramic silicone rubber cable, although the ceramic silicone rubber cable has good wear resistance, the cable manufacturing process needs special mixing, extruding and vulcanizing equipment, the process is complex, and the balance among the strength of an insulating layer, flame retardance and shielding property is difficult to achieve, so that the wear-resistant tear-resistant silicone rubber wire cable with good shielding property is researched and prepared by the invention.
Disclosure of Invention
The invention aims to provide a wear-resistant tear-resistant silicone rubber wire and cable and a preparation method thereof, so as to solve the problems in the background technology.
A wear-resistant tear-resistant silicon rubber wire cable comprises a conductor, an insulating layer, a shielding layer and a sheath layer, wherein the conductor is a copper conductor prepared by twisting single crystal copper wires; the insulating layer and the sheath layer are made of ceramic silicon rubber; the shielding layer is polyamide aerogel.
Preferably, the ceramic silicone rubber is prepared by taking methyl vinyl silicone rubber as a base body, wollastonite as a ceramic filler, self-made glass powder as a fluxing agent and fumed silica as a reinforcing agent.
Preferably, the self-made glass powder comprises calcium carbonate, zinc oxide, boric acid, ammonium dihydrogen phosphate and ammonium polyphosphate microspheres; the ammonium polyphosphate microspheres are prepared by taking carbon microspheres as core materials and ammonium polyphosphate as a shell and coating the shell with epoxy polysiloxane at two ends.
Preferably, the polyamide aerogel is prepared by introducing melamine into a polyamide main chain and adding modified multi-wall carbon nanotubes; the modified multi-walled carbon nanotube is prepared by grafting polyaryletherketone on the surface of the multi-walled carbon nanotube.
Preferably, the preparation method of the wear-resistant tear-resistant silicone rubber wire and cable comprises the following specific steps:
(1) putting the single crystal copper wire into a stranding machine for stranding to obtain a conductor; mixing the pretreated carbon microspheres, ammonium polyphosphate and deionized water according to the mass ratio of 1: 1-1: 1.2, heating to 65-75 ℃, uniformly stirring, adding double-end epoxy polysiloxane with the mass being 5-8 times that of the carbon microspheres, carrying out reflux reaction on the mixture for 2-4 hours by using absolute ethyl alcohol, cooling to room temperature, filtering, and washing for 3-5 times by using the deionized water to obtain ammonium polyphosphate microspheres;
(2) drying calcium carbonate, zinc oxide, boric acid, ammonium dihydrogen phosphate and ammonium polyphosphate microspheres, mixing according to a mass ratio of 10:40:8:35: 10-10: 50:18:35:10, carrying out homogenization mixing by using a ball mill, transferring to a crucible, melting at 1300-1500 ℃ for 1-2 h, pouring into deionized water for quenching, finally adding a dispersant, namely absolute ethyl alcohol, carrying out ball milling again, and carrying out ball milling for 24-48 h to obtain self-made glass powder;
(3) mixing methyl vinyl silicone rubber and fumed silica in a mass ratio of 2: 1-2.2: 1, placing the mixture in a vacuum kneading machine, kneading for 4-6 min, adding aluminum hydroxide 0.2-0.3 time of the mass of the methyl vinyl silicone rubber and self-made glass powder 0.3-0.35 time of the mass of the methyl vinyl silicone rubber, uniformly stirring, heating to 170-180 ℃, cooking for 80-100 min, vacuumizing to-0.06- -0.08MPa, and continuously extruding and wrapping the mixture on a conductor under the action of a forming mold and extrusion pressure to form a wire cable with an insulating layer after vacuumizing for 30-50 min;
(4) mixing poly (aryl ether ketone azide) and a multi-walled carbon nanotube according to a mass ratio of 5: 1-8: 1, placing the mixture in N-methylpyrrolidone 25-30 times of the mass of the multi-walled carbon nanotube, heating the mixture to 125-130 ℃ in a nitrogen atmosphere, reacting for 96-98 hours, cooling to room temperature, performing suction filtration, washing for 3-5 times by using N-methylpyrrolidone and deionized water in sequence, and drying in a vacuum drying oven to obtain a modified multi-walled carbon nanotube;
(5) mixing melamine and dimethyl sulfoxide according to the mass ratio of 1: 8-1: 10, adding an isophthaloyl dichloride solution with the mass of 0.2-0.4 times that of the dimethyl sulfoxide, stirring and reacting at 30-50 rpm for 30-50 min, adding a modified multi-walled carbon nanotube with the mass of 0.08-0.1 time that of the dimethyl sulfoxide, heating to 60-70 ℃, continuing to stir and react for 20-30 min, sealing and placing in a drying oven with the temperature of 40-60 ℃, taking out after 2-3 h, immersing a cable with an insulating layer, transferring to a freeze dryer with the temperature of-70-80 ℃ for freeze drying, taking out and polishing to obtain the wire cable with the shielding layer;
(6) and (4) continuously extruding and wrapping the electric wire and cable with the shielding layer on the conductor under the action of the forming die and the extrusion pressure in the step (3) to form the electric wire and cable with the sheath layer, so as to prepare the wear-resistant tear-resistant silicone rubber electric wire and cable.
Preferably, in the step (1): the preparation method of the pretreated carbon microspheres comprises the following steps: mixing and stirring glucose and deionized water according to a mass ratio of 1: 13-1: 15 until the glucose and the deionized water are dissolved, transferring the mixture into a reaction kettle, heating to 280-300 ℃, reacting for 8-10 h, cooling to room temperature, carrying out suction filtration, washing for 3-5 times by using absolute ethyl alcohol and deionized water in sequence, and finally drying in an oven at 80-90 ℃ for 12-24 h to prepare carbon microspheres; mixing and sealing the carbon microspheres, gamma-aminopropyltriethoxysilane and absolute ethyl alcohol according to the mass ratio of 1:0.2: 40-1: 0.4:50, heating to 40-45 ℃, and performing ultrasonic treatment at 50-80 kHz for 30-50 min to obtain the pretreated carbon microspheres.
Preferably, in the step (1): the preparation method of the epoxy-terminated polysiloxane comprises the following steps: mixing 1, 2-epoxy-9-decene and 2% of Kanst catalyst in a mass ratio of 1: 0.008-1: 0.01, stirring uniformly under an oil bath at 70-80 ℃, dropwise adding double-end hydrogen-containing polysiloxane with the mass of 6.3-6.6 times of that of 1, 2-epoxy-9-decene at the speed of 3-5 ml/min, reacting for 8-10 hours, adding propargyl alcohol with the mass of 1.4-1.6 times of that of 1, 2-epoxy-9-decene, stirring at room temperature and 30-50 rpm, reacting for 1.5-2.5 hours, and centrifuging to obtain a supernatant, namely the double-end epoxy polysiloxane.
Preferably, in the step (2): the preparation method of the azidation polyaryletherketone comprises the following steps: dispersing polyaryletherketone in chloroform with the mass of 8-10 times that of the polyaryletherketone in a nitrogen atmosphere, heating the solution to 80-85 ℃ in an oil bath, performing reflux reaction for 10-12 h, discharging the product in absolute ethyl alcohol, and washing the product for 3-5 times by using the absolute ethyl alcohol to obtain brominated polyaryletherketone; mixing brominated polyaryletherketone with sodium azide of which the mass is 0.08-0.1 time that of the brominated polyaryletherketone, dispersing the mixture in N-methylpyrrolidone of which the mass is 8-10 times that of the brominated polyaryletherketone, heating the mixture to 45-48 ℃ in an oil bath under the nitrogen atmosphere, reacting for 48 hours, filtering, washing for 3-5 times by deionized water and absolute ethyl alcohol in sequence, and drying for 12-15 hours at the temperature of 30-50 ℃ in a vacuum drying oven to obtain the azido polyaryletherketone.
Preferably, in the step (5): the isophthaloyl dichloride solution is an N-methyl pyrrolidone solution of isophthaloyl dichloride with the mass fraction of 3-5%.
Preferably, in the above steps (3), (5) and (6): the thickness of the insulating layer and the sheath layer is 0.15-0.25 mm; the thickness of the shielding layer is 0.1-0.2 mm.
Compared with the prior art, the invention has the following beneficial effects:
the wear-resistant tear-resistant silicone rubber wire cable comprises a conductor, an insulating layer, a shielding layer and a sheath layer; wherein the insulating layer and the sheath layer are made of ceramic silicon rubber, and the shielding layer is made of polyamide aerogel;
the ceramic silicon rubber is prepared by taking methyl vinyl silicone rubber as a substrate, wollastonite as a ceramic filler, self-made glass powder as a fluxing agent and fumed silica as a reinforcing agent; the self-made glass powder comprises calcium carbonate, zinc oxide, boric acid, ammonium dihydrogen phosphate and ammonium polyphosphate microspheres; the ammonium polyphosphate microspheres are prepared by taking carbon microspheres as core materials and ammonium polyphosphate as a shell and coating the shell with epoxy polysiloxane at two ends; the agglomeration of the carbon microspheres is reduced, the flame retardance of the modified glass powder is enhanced, gaps generated after the silicon rubber is heated and decomposed are filled by the self-made glass powder through flowing migration during melting, the polysiloxane on the surface is connected with the silicon rubber through hydrogen bonds, the density and the strength are high after the wire and cable are made into porcelain, and the strength of the wire and cable after the wire and cable are made into porcelain is enhanced;
the polyamide aerogel is prepared by introducing melamine into a polyamide main chain and adding modified multi-walled carbon nanotubes; the modified multi-walled carbon nanotube is prepared by grafting polyaryletherketone on the surface of the multi-walled carbon nanotube; polyaryletherketone with azide groups is grafted on the surface of the multi-walled carbon nanotube, the azide groups can react with double bonds to connect the polyaryletherketone on the surface, so that the dispersibility is enhanced, and nitrogen heterocycles generated on the surface can be introduced into polyamide; and then adding the modified multi-walled carbon nanotubes into polyamide as a filler, connecting the filler into the polyamide under the action of melamine to enhance the tear resistance of the shielding layer, and finally performing freeze drying to ensure that electromagnetic waves can be absorbed by times and simultaneously reflected in holes in the shielding layer, thereby enhancing the shielding performance of the shielding layer.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In order to more clearly illustrate the method provided by the invention, the following examples are used for describing the method in detail, and the test methods of each index of the abrasion-resistant tear-resistant silicone rubber wire and cable prepared in the examples and the comparative examples are as follows:
flame retardancy: the examples and comparative examples are subjected to a limiting oxygen index test with reference to GB/T2406;
and (3) tearing resistance: the examples and the comparative examples are tested for elongation at break and tensile strength after ceramization with reference to GB/T2951;
shielding property: the examples and comparative examples were tested for electromagnetic wave shielding effectiveness with reference to GB/T30142.
Example 1
(1) Putting the single crystal copper wire into a stranding machine for stranding to obtain a conductor; mixing and stirring glucose and deionized water according to a mass ratio of 1:13 until the glucose and the deionized water are dissolved, transferring the mixture into a reaction kettle, heating the mixture to 280 ℃ for reaction for 8 hours, cooling the mixture to room temperature, carrying out suction filtration, washing the mixture for 3 times by using absolute ethyl alcohol and deionized water in sequence, and finally drying the mixture for 12 hours in an oven at 80 ℃ to prepare carbon microspheres; mixing and sealing the carbon microspheres, gamma-aminopropyltriethoxysilane and absolute ethyl alcohol according to the mass ratio of 1:0.2:40, heating to 40 ℃, and performing ultrasonic treatment for 30min at 50kHz to prepare pretreated carbon microspheres; mixing 1, 2-epoxy-9-decene and 2% of Kaster catalyst according to the mass ratio of 1:0.008, stirring uniformly under an oil bath at 70 ℃, dropwise adding double-end hydrogen-containing polysiloxane with the mass 6.3 times of that of 1, 2-epoxy-9-decene at the speed of 3ml/min, reacting for 8 hours, adding propargyl alcohol with the mass 1.4 times of that of 1, 2-epoxy-9-decene, stirring at room temperature and 30rpm, reacting for 1.5 hours, and centrifuging to obtain a supernatant, namely double-end epoxy polysiloxane; mixing the pretreated carbon microspheres, ammonium polyphosphate and deionized water according to the mass ratio of 1:1, heating to 65 ℃, uniformly stirring, adding double-ended epoxy polysiloxane with the mass 5 times that of the carbon microspheres, carrying out reflux reaction on the mixture for 2 hours by using absolute ethyl alcohol, cooling to room temperature, filtering, and washing for 3 times by using the deionized water to obtain ammonium polyphosphate microspheres;
(2) dispersing polyaryletherketone in chloroform with the mass of 8 times that of the polyaryletherketone in a nitrogen atmosphere, heating in an oil bath to 80 ℃, performing reflux reaction for 10 hours, discharging in absolute ethanol, and washing with the absolute ethanol for 3 times to obtain brominated polyaryletherketone; mixing brominated polyaryletherketone with sodium azide of which the mass is 0.08 times that of the brominated polyaryletherketone, dispersing the mixture in N-methylpyrrolidone of which the mass is 8 times that of the brominated polyaryletherketone, heating the mixture in an oil bath to 45 ℃ under the nitrogen atmosphere, reacting for 48 hours, filtering, washing for 3 times by deionized water and absolute ethyl alcohol in sequence, and drying for 12 hours at the temperature of 30 ℃ in a vacuum drying oven to obtain the azido polyaryletherketone; drying calcium carbonate, zinc oxide, boric acid, ammonium dihydrogen phosphate and ammonium polyphosphate microspheres, mixing according to a mass ratio of 10:40:8:35:10, carrying out uniform mixing by using a ball mill, transferring into a crucible, melting at 1300 ℃ for 1h, pouring into deionized water for quenching, adding a dispersant, namely absolute ethyl alcohol, carrying out ball milling again, and carrying out ball milling for 24h to obtain self-made glass powder;
(3) mixing methyl vinyl silicone rubber and fumed silica in a mass ratio of 2:1, placing the mixture in a vacuum kneading machine, kneading the mixture for 4min, adding aluminum hydroxide which is 0.2 times of the mass of the methyl vinyl silicone rubber and self-made glass powder which is 0.3 times of the mass of the methyl vinyl silicone rubber, uniformly stirring the mixture, heating the mixture to 170 ℃, cooking the mixture for 80min, vacuumizing the mixture to-0.06 MPa, and continuously extruding and wrapping the mixture on a conductor under the action of a forming die and extrusion pressure to form a wire cable with an insulating layer after vacuumizing the mixture for 30 min;
(4) mixing poly (aryl ether ketone azide) and a multi-walled carbon nanotube according to a mass ratio of 5:1, placing the mixture into N-methyl pyrrolidone 25 times of the mass of the multi-walled carbon nanotube, reacting for 96 hours under the nitrogen atmosphere due to heating to 125 ℃, cooling to room temperature, performing suction filtration, washing for 3 times by sequentially using N-methyl pyrrolidone and deionized water, and drying in a vacuum drying oven to obtain a modified multi-walled carbon nanotube;
(5) mixing melamine and dimethyl sulfoxide according to a mass ratio of 1:8, adding an isophthaloyl chloride solution with the mass being 0.2 time that of the dimethyl sulfoxide, wherein the isophthaloyl chloride solution is an N-methyl pyrrolidone solution of isophthaloyl chloride with the mass fraction being 3%, stirring at 30rpm for reaction for 30min, adding a modified multi-walled carbon nanotube with the mass being 0.08 time that of the dimethyl sulfoxide, heating to 60 ℃, continuing to stir for reaction for 20min, sealing and placing in a drying oven with the temperature of 40 ℃, taking out after 2h, immersing a cable with an insulating layer, transferring to a freeze dryer with the temperature of-70 ℃ for freeze drying, taking out and polishing to obtain the wire and cable with the shielding layer;
(6) and (4) continuously extruding and wrapping the electric wire and cable with the shielding layer on the conductor under the action of the forming die and the extrusion pressure in the step (3) to form the electric wire and cable with the sheath layer, wherein the thicknesses of the insulating layer and the sheath layer are 0.15mm, and the thickness of the shielding layer is 0.1mm, so as to prepare the wear-resistant tear-resistant silicone rubber electric wire and cable.
Example 2
(1) Putting the single crystal copper wire into a stranding machine for stranding to obtain a conductor; mixing and stirring glucose and deionized water according to a mass ratio of 1:14 until the glucose and the deionized water are dissolved, transferring the mixture into a reaction kettle, heating the mixture to 290 ℃, reacting for 9 hours, cooling the mixture to room temperature, carrying out suction filtration, washing the mixture for 4 times by using absolute ethyl alcohol and deionized water in sequence, and finally drying the mixture for 46 hours in an oven at 85 ℃ to prepare carbon microspheres; mixing and sealing the carbon microspheres, gamma-aminopropyltriethoxysilane and absolute ethyl alcohol according to the mass ratio of 1:0.3:45, heating to 43 ℃, and performing ultrasonic treatment at 65kHz for 40min to obtain pretreated carbon microspheres; mixing 1, 2-epoxy-9-decene and 2% of Kanst catalyst in a mass ratio of 1:0.009, stirring uniformly under an oil bath at 75 ℃, dropwise adding hydrogen-containing polysiloxane with double ends, 6.5 times of the mass of the 1, 2-epoxy-9-decene, reacting for 9 hours at a speed of 4ml/min, adding propargyl alcohol with 1.5 times of the mass of the 1, 2-epoxy-9-decene, stirring at room temperature and 40rpm for reacting for 2 hours, and centrifuging to obtain a supernatant, namely the epoxy polysiloxane with double ends; mixing the pretreated carbon microspheres, ammonium polyphosphate and deionized water according to the mass ratio of 1:1.1, heating to 70 ℃, uniformly stirring, adding double-ended epoxy polysiloxane with the mass 6 times that of the carbon microspheres, carrying out reflux reaction on the mixture for 3 hours by using absolute ethyl alcohol, cooling to room temperature, filtering, and washing for 4 times by using the deionized water to obtain ammonium polyphosphate microspheres;
(2) dispersing polyaryletherketone in chloroform 9 times the weight of polyaryletherketone in nitrogen atmosphere, heating to 83 ℃ in an oil bath, performing reflux reaction for 11h, discharging in absolute ethyl alcohol, and washing with absolute ethyl alcohol for 4 times to obtain brominated polyaryletherketone; mixing brominated polyaryletherketone with sodium azide of which the mass is 0.09 times that of the brominated polyaryletherketone, dispersing the mixture in N-methylpyrrolidone of which the mass is 9 times that of the brominated polyaryletherketone, heating the mixture in an oil bath to 46 ℃ in a nitrogen atmosphere, reacting for 48 hours, filtering, washing for 4 times by deionized water and absolute ethyl alcohol in sequence, and drying for 14 hours at the temperature of 40 ℃ in a vacuum drying oven to obtain the azido polyaryletherketone; drying calcium carbonate, zinc oxide, boric acid, ammonium dihydrogen phosphate and ammonium polyphosphate microspheres, mixing according to a mass ratio of 10:45:12:35:10, carrying out uniform mixing by using a ball mill, transferring into a crucible, melting at 1400 ℃ for 1.5h, pouring into deionized water for quenching, finally adding a dispersant, namely absolute ethyl alcohol, carrying out ball milling again, and carrying out ball milling for 36h to obtain self-made glass powder;
(3) mixing methyl vinyl silicone rubber and fumed silica in a mass ratio of 2.1:1, placing the mixture in a vacuum kneading machine, kneading the mixture for 5min, adding aluminum hydroxide which is 0.25 times of the mass of the methyl vinyl silicone rubber and self-made glass powder which is 0.32 times of the mass of the methyl vinyl silicone rubber, uniformly stirring the mixture, heating the mixture to 175 ℃, cooking the mixture for 90min, vacuumizing the mixture to-0.07 MPa, and continuously extruding and wrapping the mixture on a conductor under the action of a forming die and extrusion pressure to form a wire cable with an insulating layer after vacuumizing the mixture for 40 min;
(4) mixing poly (aryl ether ketone azide) and a multi-walled carbon nanotube according to a mass ratio of 6:1, placing the mixture into N-methyl pyrrolidone 27 times the mass of the multi-walled carbon nanotube, reacting for 97 hours under the nitrogen atmosphere as the mixture is heated to 128 ℃, cooling to room temperature, performing suction filtration, washing for 4 times by sequentially using N-methyl pyrrolidone and deionized water, and drying in a vacuum drying oven to obtain a modified multi-walled carbon nanotube;
(5) mixing melamine and dimethyl sulfoxide according to a mass ratio of 1:9, adding an isophthaloyl chloride solution with the mass being 0.3 time of that of the dimethyl sulfoxide, wherein the isophthaloyl chloride solution is an N-methylpyrrolidone solution of isophthaloyl chloride with the mass fraction of 4%, stirring and reacting at 40rpm for 40min, adding a modified multi-walled carbon nanotube with the mass being 0.09 time of that of the dimethyl sulfoxide, heating to 65 ℃, continuing to stir and react for 25min, sealing and placing in a 50 ℃ drying oven, taking out after 2.5h, immersing a cable with an insulating layer, transferring to a-75 ℃ freeze dryer for freeze drying, taking out and polishing to obtain the wire and cable with a shielding layer;
(6) and (4) continuously extruding and wrapping the electric wire and cable with the shielding layer on the conductor under the action of the forming die and the extrusion pressure in the step (3) to form the electric wire and cable with the sheath layer, wherein the thicknesses of the insulating layer and the sheath layer are 0.2mm, and the thickness of the shielding layer is 0.15mm, so as to prepare the wear-resistant tear-resistant silicone rubber electric wire and cable.
Example 3
(1) Putting the single crystal copper wire into a stranding machine for stranding to obtain a conductor; mixing and stirring glucose and deionized water according to a mass ratio of 1:15 until the glucose and the deionized water are dissolved, transferring the mixture into a reaction kettle, heating the mixture to 300 ℃, reacting the mixture for 10 hours, cooling the mixture to room temperature, carrying out suction filtration, washing the mixture for 5 times by using absolute ethyl alcohol and deionized water in sequence, and finally drying the mixture for 24 hours in a drying oven at 90 ℃ to prepare carbon microspheres; mixing and sealing the carbon microspheres, gamma-aminopropyltriethoxysilane and absolute ethyl alcohol according to the mass ratio of 1:0.4:50, heating to 45 ℃, and carrying out ultrasonic treatment for 50min at 80kHz to obtain pretreated carbon microspheres; mixing 1, 2-epoxy-9-decene and 2% of Kanst catalyst in a mass ratio of 1:0.01, stirring uniformly under an oil bath at 80 ℃, dropwise adding double-end hydrogen-containing polysiloxane with the mass of 6.6 times of that of the 1, 2-epoxy-9-decene at a speed of 5ml/min, reacting for 10 hours, adding propargyl alcohol with the mass of 1.6 times of that of the 1, 2-epoxy-9-decene, stirring at room temperature and 50rpm, reacting for 2.5 hours, and centrifuging to obtain a supernatant, namely the double-end epoxy polysiloxane; mixing the pretreated carbon microspheres, ammonium polyphosphate and deionized water according to the mass ratio of 1:1.2, heating to 75 ℃, uniformly stirring, adding double-ended epoxy polysiloxane with the mass being 8 times that of the carbon microspheres, carrying out reflux reaction on the mixture for 4 hours by using absolute ethyl alcohol, cooling to room temperature, filtering, and washing the mixture for 5 times by using the deionized water to obtain ammonium polyphosphate microspheres;
(2) dispersing polyaryletherketone in chloroform with the mass of 10 times that of the polyaryletherketone in nitrogen atmosphere, heating to 85 ℃ in an oil bath, performing reflux reaction for 12 hours, discharging in absolute ethyl alcohol, and washing for 5 times by using the absolute ethyl alcohol to obtain brominated polyaryletherketone; mixing brominated polyaryletherketone with sodium azide of which the mass is 0.1 time that of the brominated polyaryletherketone, dispersing the mixture in N-methylpyrrolidone of which the mass is 8-10 times that of the brominated polyaryletherketone, heating the mixture in an oil bath to 48 ℃ in a nitrogen atmosphere, reacting for 48 hours, filtering, washing for 5 times by using deionized water and absolute ethyl alcohol in sequence, and drying for 15 hours in a vacuum drying oven at 50 ℃ to obtain the azido polyaryletherketone; drying calcium carbonate, zinc oxide, boric acid, ammonium dihydrogen phosphate and ammonium polyphosphate microspheres, mixing according to a mass ratio of 10:50:18:35:10, carrying out uniform mixing by using a ball mill, transferring into a crucible, melting at 1500 ℃ for 2 hours, pouring into deionized water for quenching, adding a dispersant, namely absolute ethyl alcohol, carrying out ball milling again, and carrying out ball milling for 48 hours to obtain self-made glass powder;
(3) mixing methyl vinyl silicone rubber and fumed silica in a mass ratio of 2.2:1, placing the mixture in a vacuum kneading machine, kneading the mixture for 6min, adding aluminum hydroxide which is 0.3 time of the mass of the methyl vinyl silicone rubber and self-made glass powder which is 0.35 time of the mass of the methyl vinyl silicone rubber, uniformly stirring the mixture, heating the mixture to 180 ℃, cooking the mixture for 100min, vacuumizing the mixture to-0.08 MPa, and continuously extruding and wrapping the mixture on a conductor under the action of a forming die and extrusion pressure to form a wire cable with an insulating layer after vacuumizing the mixture for 50 min;
(4) mixing poly aryl ether ketone azide and a multi-walled carbon nanotube according to a mass ratio of 8:1, placing the mixture into N-methyl pyrrolidone with the mass of 30 times that of the multi-walled carbon nanotube, heating the mixture to 130 ℃ in a nitrogen atmosphere, reacting for 98 hours, cooling the mixture to room temperature, performing suction filtration, washing the mixture for 5 times by using N-methyl pyrrolidone and deionized water in sequence, and drying the mixture in a vacuum drying oven to obtain a modified multi-walled carbon nanotube;
(5) mixing melamine and dimethyl sulfoxide according to a mass ratio of 1:10, adding an isophthaloyl chloride solution with the mass being 0.4 time that of the dimethyl sulfoxide, wherein the isophthaloyl chloride solution is an N-methyl pyrrolidone solution of isophthaloyl chloride with the mass fraction of 5%, stirring at 50rpm for reaction for 50min, adding a modified multi-walled carbon nanotube with the mass being 0.1 time that of the dimethyl sulfoxide, heating to 70 ℃, continuing to stir for reaction for 30min, sealing in a 60 ℃ oven, taking out after 3h, immersing a cable with an insulating layer, transferring to a-80 ℃ freeze dryer for freeze drying, taking out and polishing to obtain the wire and cable with a shielding layer;
(6) and (4) continuously extruding and wrapping the electric wire and cable with the shielding layer on the conductor under the action of the forming die and the extrusion pressure in the step (3) to form the electric wire and cable with the sheath layer, wherein the thicknesses of the insulating layer and the sheath layer are 0.25mm, and the thickness of the shielding layer is 0.2mm, so as to prepare the wear-resistant tear-resistant silicone rubber electric wire and cable.
Comparative example 1
The formulation of comparative example 1 was the same as that of example 2. The wear-resistant tear-resistant silicone rubber wire and cable and the preparation method thereof are different from the embodiment 2 only in the difference of the step (1), and the step (1) is modified as follows: placing kaolin in a calcining furnace, heating to 825 ℃, and calcining for 2 hours to prepare metakaolin; mixing metakaolin, alkaline residue, water and grinding aid triethanolamine according to a mass ratio of 13:7:5.5:0.15, and then feeding the mixture into a wet ball mill for grinding to prepare a heat-preservation slurry blank; mixing the heat-preservation slurry blank with 85% phosphoric acid in a mass ratio of 26:7, placing the mixture in a constant temperature tank at 3 ℃, and stirring for 30min at a temperature of 500rpm to obtain the heat-preservation slurry.
Comparative example 2
Comparative example 2 was formulated in the same manner as in example 2. The wear-resistant tear-resistant silicone rubber wire and cable and the preparation method thereof are different from the embodiment 2 only in the difference of the step (2), and the step (1) is modified as follows: mixing hydrogen-containing silicone oil and allyl glycidyl ether according to the mass ratio of 1:2.2, uniformly stirring, heating to 73 ℃, adding a catalyst which is a chloroplatinic acid ethanol solution with the mass fraction of 3% and accounts for 0.5 time of the mass of the hydrogen-containing silicone oil, reacting for 15min, heating to 83 ℃, reacting for 6h, and carrying out vacuum distillation to obtain epoxy hydrogen-containing silicone oil; mixing epoxy hydrogen-containing silicone oil, 3-hydroxypropionic acid, a catalyst potassium hydroxide and a polymerization inhibitor p-hydroxyanisole according to a mass ratio of 1.1:1.3:0.07, heating to 100 ℃, reacting for 6 hours, washing for 4 times by using a saturated sodium carbonate solution and deionized water in sequence, and drying by using anhydrous magnesium sulfate to obtain the hyperbranched organosilicon.
Comparative example 3
The formulation of comparative example 3 was the same as example 2. The wear-resistant tear-resistant silicone rubber wire and cable and the preparation method thereof are different from those in the embodiment 2 only in the difference of the step (2), and the step (2) is modified as follows: mixing hydrogen-containing silicone oil and allyl glycidyl ether according to the mass ratio of 1:2.2, uniformly stirring, heating to 73 ℃, adding a catalyst which is 0.5 time of the mass of the hydrogen-containing silicone oil, wherein the catalyst is a chloroplatinic acid ethanol solution with the mass fraction of 3%, reacting for 15min, heating to 83 ℃, reacting for 6h, and carrying out vacuum distillation to obtain epoxy hydrogen-containing silicone oil; mixing ethoxytrimethylsilane, vinyltriethoxysilane, deionized water and toluene according to the mass ratio of 1.1:4.1:6:2.5, heating to 55 ℃, reacting for 3.5h, dropwise adding hydrochloric acid with the mass fraction of 6% and the mass of 0.5 time of that of the toluene at the speed of 4ml/min, reacting for 2.5h under heat preservation, washing for 4 times by using a saturated sodium carbonate solution and deionized water in sequence, drying by using anhydrous magnesium sulfate, and distilling under reduced pressure at 128 ℃ and 10kPa to prepare branched-chain silane; adding branched chain type silane which is 1.3 times of the weight of the epoxy hydrogen-containing silicone oil and hydrochloric acid which is 0.3 times of the weight of the epoxy hydrogen-containing silicone oil and has the mass fraction of 6% into the epoxy hydrogen-containing silicone oil, keeping the temperature at 100 ℃ for reaction for 4 hours, washing the mixture for 4 times by using saturated sodium carbonate solution and deionized water in sequence, and drying the mixture by using anhydrous magnesium sulfate to prepare the hyperbranched silicone.
Comparative example 4
Comparative example 4 was formulated as in example 2. The abrasion-resistant tear-resistant silicone rubber wire and cable and the preparation method thereof are only different from the embodiment 2 in that the treatment of the step (2) is not carried out, and the step (3) is modified as follows: mixing styrene, butyl acrylate, acrylic acid, water and an emulsifier OP-10, stirring at 150rpm for 40min, adding an initiator potassium persulfate and an ammonium bicarbonate solution with the mass fraction of 8%, heating to 90 ℃, reacting for 4h, cooling to room temperature, adjusting the pH to 7.4 with ammonia water, and filtering to prepare a styrene-acrylic emulsion, wherein the mass ratio of the initiator potassium persulfate to the ammonium bicarbonate solution is 19:29:2.2:50:0.9:0.8: 18; and a styrene-acrylic emulsion is used in the step (4).
Examples of effects
Table 1 below shows the results of performance analysis of abrasion and tear resistant silicone rubber wire and cable using examples 1,2, 3 and comparative examples 1,2, 3 and 4 of the present invention.
TABLE 1
| Oxygen index (%) | Tensile strength (N/mm) 2 ) | Elongation at Break (%) | Electromagnetic shield (dB) | |
| Example 1 | 42 | 163 | 253 | 62 |
| Example 2 | 42 | 167 | 254 | 65 |
| Example 3 | 41 | 158 | 249 | 64 |
| Comparative example 1 | 40 | 143 | 224 | 60 |
| Comparative example 2 | 35 | 139 | 218 | 61 |
| Comparative example 3 | 39 | 156 | 245 | 55 |
| Comparative example 4 | 40 | 157 | 247 | 52 |
Compared with the experimental data of the comparative example and the examples in the table 1, it can be obviously found that the abrasion-resistant tear-resistant silicone rubber wire and cable prepared in the examples 1,2 and 3 have better flame retardance, tear resistance and shielding property;
from the comparison of the experimental data of examples 1,2 and 3 and comparative examples 1 and 2, it can be seen that self-made glass powder is used as a fluxing agent when preparing the ceramic silicon rubber, and the self-made glass powder comprises calcium carbonate, zinc oxide, boric acid, ammonium dihydrogen phosphate and ammonium polyphosphate microspheres; the surfaces of the ammonium polyphosphate microspheres are coated with double-end epoxy polysiloxane, so that the flame retardance of the wire and cable is enhanced, the wire and cable has high density and strength after being made into porcelain, and the strength of the wire and cable after being made into porcelain is enhanced; from a comparison of the experimental data of examples 1,2, 3 and comparative examples 3, 4, it can be seen that the introduction of melamine and the use of multi-walled carbon nanotubes with surface grafted polyaryletherketone in the polyamide aerogel can enhance the tear resistance and barrier properties of the barrier layer.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (10)
1. A wear-resistant tear-resistant silicone rubber wire cable comprises a conductor, an insulating layer, a shielding layer and a sheath layer, and is characterized in that the conductor is a copper conductor prepared by twisting single crystal copper wires; the insulating layer and the sheath layer are made of ceramic silicon rubber; the shielding layer is polyamide aerogel.
2. The wear-resistant tear-resistant silicone rubber wire and cable of claim 1, wherein the ceramic silicone rubber is prepared by using methyl vinyl silicone rubber as a base, wollastonite as a ceramic filler, self-made glass powder as a fluxing agent, and fumed silica as a reinforcing agent.
3. The wear-resistant tear-resistant silicone rubber wire and cable as claimed in claim 2, wherein the self-made glass powder comprises calcium carbonate, zinc oxide, boric acid, ammonium dihydrogen phosphate and ammonium polyphosphate microspheres; the ammonium polyphosphate microspheres are prepared by taking carbon microspheres as core materials and ammonium polyphosphate as a shell and coating the shell with epoxy polysiloxane at two ends.
4. The abrasion-resistant tear-resistant silicone rubber wire and cable as claimed in claim 1, wherein the polyamide aerogel is prepared by introducing melamine into a polyamide main chain and adding modified multi-walled carbon nanotubes; the modified multi-walled carbon nanotube is prepared by grafting polyaryletherketone on the surface of the multi-walled carbon nanotube.
5. The preparation method of the wear-resistant tear-resistant silicone rubber wire and cable is characterized by comprising the following specific steps:
(1) putting the single crystal copper wire into a stranding machine for stranding to obtain a conductor; mixing the pretreated carbon microspheres, ammonium polyphosphate and deionized water according to the mass ratio of 1: 1-1: 1.2, heating to 65-75 ℃, uniformly stirring, adding double-end epoxy polysiloxane with the mass being 5-8 times that of the carbon microspheres, carrying out reflux reaction on absolute ethyl alcohol for 2-4 hours, cooling to room temperature, filtering, and washing with deionized water for 3-5 times to obtain ammonium polyphosphate microspheres;
(2) drying calcium carbonate, zinc oxide, boric acid, ammonium dihydrogen phosphate and ammonium polyphosphate microspheres, mixing according to a mass ratio of 10:40:8:35: 10-10: 50:18:35:10, uniformly mixing by using a ball mill, transferring into a crucible, melting at 1300-1500 ℃ for 1-2 hours, pouring into deionized water for quenching, adding a dispersant, namely absolute ethyl alcohol, and performing ball milling again for 24-48 hours to prepare self-made glass powder;
(3) mixing methyl vinyl silicone rubber and fumed silica in a mass ratio of 2: 1-2.2: 1, placing the mixture in a vacuum kneading machine, kneading for 4-6 min, adding aluminum hydroxide 0.2-0.3 time of the mass of the methyl vinyl silicone rubber and self-made glass powder 0.3-0.35 time of the mass of the methyl vinyl silicone rubber, uniformly stirring, heating to 170-180 ℃, cooking for 80-100 min, vacuumizing to-0.06- -0.08MPa, and continuously extruding and wrapping the mixture on a conductor under the action of a forming mold and extrusion pressure to form a wire cable with an insulating layer after vacuumizing for 30-50 min;
(4) mixing poly (aryl ether ketone azide) and a multi-walled carbon nanotube according to a mass ratio of 5: 1-8: 1, placing the mixture in N-methylpyrrolidone 25-30 times of the mass of the multi-walled carbon nanotube, heating the mixture to 125-130 ℃ in a nitrogen atmosphere, reacting for 96-98 hours, cooling to room temperature, performing suction filtration, washing for 3-5 times by using N-methylpyrrolidone and deionized water in sequence, and drying in a vacuum drying oven to obtain a modified multi-walled carbon nanotube;
(5) mixing melamine and dimethyl sulfoxide according to the mass ratio of 1: 8-1: 10, adding an isophthaloyl dichloride solution with the mass of 0.2-0.4 times that of the dimethyl sulfoxide, stirring and reacting at 30-50 rpm for 30-50 min, adding a modified multi-walled carbon nanotube with the mass of 0.08-0.1 time that of the dimethyl sulfoxide, heating to 60-70 ℃, continuing to stir and react for 20-30 min, sealing and placing in a drying oven with the temperature of 40-60 ℃, taking out after 2-3 h, immersing a cable with an insulating layer, transferring to a freeze dryer with the temperature of-70-80 ℃ for freeze drying, taking out and polishing to obtain the wire cable with the shielding layer;
(6) and (4) continuously extruding and wrapping the electric wire and cable with the shielding layer on the conductor under the action of the forming die and the extrusion pressure in the step (3) to form the electric wire and cable with the sheath layer, so as to prepare the wear-resistant tear-resistant silicone rubber electric wire and cable.
6. The method for preparing the abrasion-resistant tear-resistant silicone rubber wire and cable according to claim 5, wherein in the step (1): the preparation method of the pretreated carbon microsphere comprises the following steps: mixing and stirring glucose and deionized water according to a mass ratio of 1: 13-1: 15 until the glucose and the deionized water are dissolved, transferring the mixture into a reaction kettle, heating the mixture to 280-300 ℃, reacting for 8-10 h, cooling the mixture to room temperature, performing suction filtration, washing the mixture for 3-5 times by using absolute ethyl alcohol and deionized water in sequence, and finally drying the mixture in an oven at 80-90 ℃ for 12-24 h to prepare carbon microspheres; mixing and sealing the carbon microspheres, gamma-aminopropyltriethoxysilane and absolute ethyl alcohol according to the mass ratio of 1:0.2: 40-1: 0.4:50, heating to 40-45 ℃, and performing ultrasonic treatment at 50-80 kHz for 30-50 min to obtain the pretreated carbon microspheres.
7. The method for preparing the abrasion-resistant tear-resistant silicone rubber wire and cable according to claim 5, wherein in the step (1): the preparation method of the epoxy-terminated polysiloxane comprises the following steps: mixing 1, 2-epoxy-9-decene and 2% of Kanst catalyst in a mass ratio of 1: 0.008-1: 0.01, stirring uniformly under an oil bath at 70-80 ℃, dropwise adding double-end hydrogen-containing polysiloxane with the mass of 6.3-6.6 times of that of 1, 2-epoxy-9-decene at the speed of 3-5 ml/min, reacting for 8-10 hours, adding propargyl alcohol with the mass of 1.4-1.6 times of that of 1, 2-epoxy-9-decene, stirring at room temperature and 30-50 rpm, reacting for 1.5-2.5 hours, and centrifuging to obtain a supernatant, namely the double-end epoxy polysiloxane.
8. The method for preparing the abrasion-resistant tear-resistant silicone rubber wire and cable according to claim 5, wherein in the step (2): the preparation method of the azidation polyaryletherketone comprises the following steps: dispersing polyaryletherketone in chloroform with the mass of 8-10 times that of the polyaryletherketone in a nitrogen atmosphere, heating the solution to 80-85 ℃ in an oil bath, performing reflux reaction for 10-12 h, discharging the product in absolute ethyl alcohol, and washing the product for 3-5 times by using the absolute ethyl alcohol to obtain brominated polyaryletherketone; mixing brominated polyaryletherketone with sodium azide of which the mass is 0.08-0.1 time that of the brominated polyaryletherketone, dispersing the mixture in N-methylpyrrolidone of which the mass is 8-10 times that of the brominated polyaryletherketone, heating the mixture to 45-48 ℃ in an oil bath under the nitrogen atmosphere, reacting for 48 hours, filtering, washing for 3-5 times by deionized water and absolute ethyl alcohol in sequence, and drying for 12-15 hours at the temperature of 30-50 ℃ in a vacuum drying oven to obtain the azido polyaryletherketone.
9. The method for preparing the abrasion-resistant tear-resistant silicone rubber wire cable according to claim 5, wherein in the step (5): the isophthaloyl dichloride solution is an N-methyl pyrrolidone solution of isophthaloyl dichloride with the mass fraction of 3-5%.
10. The method for preparing a wear-resistant tear-resistant silicone rubber wire cable according to claim 5, wherein in the steps (3) (5) (6): the thickness of the insulating layer and the sheath layer is 0.15-0.25 mm; the thickness of the shielding layer is 0.1-0.2 mm.
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| CN116655964B (en) * | 2023-06-30 | 2024-03-29 | 江苏普非尔塑料科技有限公司 | High-weather-resistance high-rigidity polyamide composite material and preparation process thereof |
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