CN113652077B - Irradiation crosslinking rubber-based flame-retardant cable and preparation method thereof - Google Patents
Irradiation crosslinking rubber-based flame-retardant cable and preparation method thereof Download PDFInfo
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- C08L75/00—Compositions of polyureas or polyurethanes; Compositions of derivatives of such polymers
- C08L75/04—Polyurethanes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
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- H01B7/00—Insulated conductors or cables characterised by their form
- H01B7/17—Protection against damage caused by external factors, e.g. sheaths or armouring
- H01B7/28—Protection against damage caused by moisture, corrosion, chemical attack or weather
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- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B7/00—Insulated conductors or cables characterised by their form
- H01B7/17—Protection against damage caused by external factors, e.g. sheaths or armouring
- H01B7/29—Protection against damage caused by extremes of temperature or by flame
- H01B7/295—Protection against damage caused by extremes of temperature or by flame using material resistant to flame
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- C08L2312/00—Crosslinking
- C08L2312/06—Crosslinking by radiation
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Abstract
The invention discloses an irradiation crosslinking rubber-based flame-retardant cable and a preparation method thereof, which relate to the technical field of cable processing, wherein the irradiation crosslinking rubber-based flame-retardant cable comprises a conductor, an insulating layer, a shielding layer, an oxygen-isolation flame-retardant layer and an outer sheath layer from inside to outside, and the outer sheath layer comprises the following raw materials in parts by weight: 60-80 parts of polyurethane rubber, 20-40 parts of ethylene propylene diene monomer rubber, 15-25 parts of modified nano boron nitride particles, 4-6 parts of carbon black, 3-8 parts of nano zinc oxide, 8-10 parts of methyl silicone oil, 10-15 parts of flame retardant, 0.4-0.6 part of antioxidant and 1-2 parts of silane coupling agent. The irradiation crosslinking rubber-based flame-retardant cable and the preparation method thereof have the advantages that the raw material formula of the outer sheath layer is designed, the irradiation crosslinking rubber-based flame-retardant cable has excellent irradiation resistance, can be suitable for irradiation crosslinking production, and the preparation process is relatively lower in energy consumption, simpler and safer.
Description
Technical Field
The invention relates to the technical field of cable processing, in particular to an irradiation crosslinking rubber-based flame-retardant cable, and a preparation method and application thereof.
Background
At present, the application range of the electric wires and cables is wider and wider, and because the insulating materials and the sheath materials of the electric wires and cables are mostly organic polymers, the electric wires and cables can be burnt at a certain temperature and oxygen concentration. The cable brings convenience to society and also brings fire risks, the cable is ignited due to self and external reasons, the cable possibly spreads from inside to outside of a building along the direction of cable laying, other combustible materials are ignited to cause larger fire, and various toxic smoke is generated when the cable burns, so that life and property losses are caused. In order to reduce the fire hazard, it is necessary to perform flame retardant treatment on the polymer used for the electric wires and cables.
The flame-retardant rubber material of the current cable is mostly prepared by adding additives such as flame retardant, vulcanizing agent and the like into natural styrene-butadiene rubber, ethylene-propylene-diene monomer, chlorinated polyethylene or chlorosulfonated polyethylene, and then putting the mixture into a high-temperature high-pressure vulcanizing pipeline for vulcanization molding. This process has several disadvantages:
1. the vulcanizing pipeline is longer, the length is 60-70 m, the length is 120-150 m, the occupied area is large, and the management is complex.
2. In the sealed steam pipeline, the production condition of the cable cannot be checked, is uncontrollable, is easy to occur under-sulfur or over-sulfur, and is difficult to control the product quality.
3. The vulcanizing process needs to use a boiler for heating, high-pressure steam is generated, equipment is complex, and safety risks are high.
4. And the power consumption and the energy consumption are high.
Therefore, how to provide a cable that can be continuously produced, has relatively low energy consumption and is safer and controllable is a problem that needs to be solved in the industry.
Disclosure of Invention
Aiming at the problems, the invention aims to design and provide the irradiation crosslinking rubber-based flame-retardant cable and the preparation method thereof, wherein the raw material formula of the outer sheath layer is designed, so that the irradiation crosslinking rubber-based flame-retardant cable has excellent irradiation resistance, can be suitable for irradiation crosslinking production, and has lower energy consumption, simpler preparation process and safety.
The invention solves the technical problems by the following technical means:
the irradiation crosslinking rubber-based flame-retardant cable comprises a conductor, an insulating layer, a shielding layer, an oxygen-insulating flame-retardant layer and an outer sheath layer from inside to outside, wherein the outer sheath layer comprises the following raw materials in parts by weight: 60-80 parts of polyurethane rubber, 20-40 parts of ethylene propylene diene monomer rubber, 15-25 parts of modified nano boron nitride particles, 4-6 parts of carbon black, 3-8 parts of nano zinc oxide, 8-10 parts of methyl silicone oil, 10-15 parts of flame retardant, 0.4-0.6 part of antioxidant and 1-2 parts of silane coupling agent.
The rubber material can absorb partial irradiation energy in the irradiation process, a large number of free radicals are generated, so that ageing is generated, the elongation at break of the material is reduced, the hardness is increased, the polyurethane rubber is adopted as a main body base material, the ethylene propylene diene monomer rubber is matched, the irradiation resistance of the outer sheath can be effectively improved, meanwhile, modified nano boron nitride particles are added, on the one hand, the modified nano boron nitride particles can serve as rigid inorganic particles to increase the mechanical property of the base material, and on the other hand, the modified nano boron nitride particles can also capture the free radicals generated by irradiation, so that ageing generated by irradiation is reduced to a certain extent, and the performance of the outer sheath is further guaranteed.
Further, the outer sheath layer comprises the following raw materials in parts by weight: 75 parts of polyurethane rubber, 30 parts of ethylene propylene diene monomer rubber, 22 parts of modified nano boron nitride particles, 5 parts of carbon black, 6 parts of nano zinc oxide, 8 parts of methyl silicone oil, 12 parts of flame retardant, 0.6 part of antioxidant and 2 parts of silane coupling agent.
Further, the modified nano boron nitride particles are obtained by grafting modification of cubic boron nitride by using 1, 1-diphenylethylene.
According to the modified nano boron nitride particle, firstly boron atoms in boron nitride are introduced, the effect of improving the irradiation resistance is achieved to a certain extent, secondly, 1-diphenylethylene is grafted and introduced to the surface of the boron nitride, the 1, 1-diphenylethylene contains two phenyl groups, the phenyl groups serve as electrophilic groups, free radicals generated by irradiation of a base material can be captured, the free radicals can be prevented from continuously reacting with other base materials, degradation and aging are caused, the irradiation resistance of an outer sheath is improved, and the limit between the base material and the modified nano boron nitride particle can be blurred through the capture of the 1, 1-diphenylethylene, so that the dispersibility of the modified nano boron nitride particle in the base material is improved.
Further, the preparation method of the modified nano boron nitride particles comprises the following steps: adding pretreated cubic boron nitride powder into toluene, stirring and dispersing, dropwise adding a coupling agent, uniformly dispersing by ultrasonic to obtain a suspension, adding phosphorus oxychloride into the suspension, stirring at room temperature for reaction for 12-14h, adding azodiisobutyronitrile and 1, 1-diphenylethylene, introducing argon into an ice salt bath for 20-30min, discharging to normal pressure, reacting at 60-80 ℃ for 6-8h at an oil bath temperature, filtering after the reaction is finished, washing a filter cake with absolute ethyl alcohol, acetone and deionized water, and drying in vacuum to obtain modified nano boron nitride particles.
And the pretreatment is to ultrasonically add the cubic boron nitride powder into hydrogen peroxide solution, heat-preserving and refluxing for 3-4 hours, filtering, washing a filter cake with deionized water, stirring and dispersing the filter cake into the deionized water, and performing low-temperature plasma treatment.
The hydrogen peroxide treatment and the low-temperature plasma treatment are carried out on the opposite boron nitride, and functional groups such as hydroxyl, carboxyl and the like are introduced into the surface of the boron nitride, so that the grafting reaction between the boron nitride and the 1, 1-diphenylethylene is facilitated.
In addition, the invention also discloses a preparation method of the irradiation crosslinking rubber-based flame-retardant cable, which specifically comprises the following steps:
s1: drawing wires of the metal, annealing and twisting to obtain a conductor;
s2: extruding the conductor by an extruding process to obtain an insulating layer;
s3: braiding the outer surface of the insulating layer to obtain a shielding layer;
s4: the shielding layer is externally wrapped by a flame-retardant wrapping tape to obtain an oxygen-isolation flame-retardant layer;
s5: and extruding the prepared outer sheath granules on the surface of the oxygen-isolation flame-retardant layer through an extruder, cooling and forming, and irradiating by using a high-energy electron accelerator to obtain a cable finished product.
Further, the parameters of the irradiation of the high-energy electron accelerator are as follows: the irradiation voltage is 1.5-2MeV, the irradiation current is 20-60mA, and the speed is 200-400m/min.
Further, the preparation method of the outer sheath granule comprises the following steps:
a1: adding polyurethane rubber and ethylene propylene diene monomer into an open mill for plasticating, then adding modified nano boron nitride particles, carbon black and nano zinc oxide, heating to 80-90 ℃, mixing for 30min, adding methyl silicone oil, a flame retardant, an antioxidant and a silane coupling agent, heating to 120-140 ℃, mixing uniformly, and tabletting for molding to obtain master batch;
a2: placing the masterbatch in an internal mixer, performing triangular package rolling treatment, uniformly mixing, then discharging, and extruding and granulating by a double-screw extruder to obtain the outer sheath granules.
Further, the temperature of the twin-screw extruder is 175-220 ℃.
The invention has the beneficial effects that:
according to the irradiation crosslinking rubber-based flame-retardant cable disclosed by the invention, the irradiation resistance of a base material is improved by taking polyurethane rubber as a main base material and ethylene propylene diene monomer rubber as an auxiliary material through designing the raw material formula of the outer sheath, and the modified nano boron nitride particles, carbon black and the like are also used as auxiliary materials, so that the outer sheath can be suitable for irradiation crosslinking production, and the preparation process parameters and the like are regulated.
Detailed Description
The present invention will be described in detail with reference to the following specific examples:
example 1
Preparation of modified nano boron nitride particles
Adding cubic boron nitride powder into hydrogen peroxide solution, carrying out ultrasonic dispersion, carrying out heat preservation and reflux for 4 hours at the temperature of 60 ℃, filtering, washing a filter cake with deionized water, stirring and dispersing in the deionized water, and carrying out low-temperature plasma treatment by taking air as working gas.
Adding pretreated cubic boron nitride powder into toluene according to a solid-to-liquid ratio of 1.5g/L, stirring and dispersing, dropwise adding a coupling agent with the mass of 0.05 times of the cubic boron nitride powder, uniformly dispersing by ultrasonic to obtain a suspension, adding phosphorus oxychloride into the suspension, stirring and reacting for 14 hours at room temperature, adding azodiisobutyronitrile and 1, 1-diphenylethylene, wherein the volume ratio of toluene, phosphorus oxychloride and azoisobutyronitrile is 8:1:0.4, the mass ratio of the cubic boron nitride powder to the 1, 1-diphenylethylene is 1:1.5, introducing argon into an ice salt bath to be pressurized to 0.3MPa, maintaining for 30 minutes, discharging to normal pressure, reacting for 6 hours at the temperature of 80 ℃, filtering after the reaction is finished, washing a filter cake by absolute ethyl alcohol, acetone and deionized water, and drying in vacuum to obtain modified nanometer boron nitride particles.
Preparation of outer sheath pellets
A1: adding 75 parts of polyurethane rubber and 30 parts of ethylene propylene diene monomer rubber into an open mill for plasticating, then adding 22 parts of modified nano boron nitride particles, 5 parts of carbon black and 6 parts of nano zinc oxide, heating to 90 ℃, mixing for 30min, adding 8 parts of methyl silicone oil, 12 parts of flame retardant, 0.6 part of antioxidant and 2 parts of silane coupling agent, heating to 140 ℃, mixing uniformly, and tabletting to obtain master batch;
a2: and (3) placing the masterbatch in an internal mixer, performing triangular package rolling treatment, uniformly mixing, then feeding the masterbatch into a piece, and extruding and granulating the masterbatch at 220 ℃ through a double-screw extruder to obtain the outer sheath granules.
Preparation of a Cable
S1: drawing wires of the metal, annealing and twisting to obtain a conductor;
s2: extruding the conductor by an extruding process to obtain an insulating layer;
s3: braiding the outer surface of the insulating layer to obtain a shielding layer;
s4: the shielding layer is externally wrapped by a flame-retardant wrapping tape to obtain an oxygen-isolation flame-retardant layer;
s5: extruding the prepared outer sheath granules on the surface of the oxygen-isolation flame-retardant layer through an extruder, cooling and molding, and irradiating with an irradiation voltage of 1.8MeV, an irradiation current of 60mA and a speed of 400m/min by using a high-energy electron accelerator to obtain a cable finished product.
Example two
Preparation of modified nano boron nitride particles
Adding cubic boron nitride powder into hydrogen peroxide solution, carrying out ultrasonic dispersion, carrying out heat preservation and reflux for 4 hours at the temperature of 60 ℃, filtering, washing a filter cake with deionized water, stirring and dispersing in the deionized water, and carrying out low-temperature plasma treatment by taking air as working gas.
Adding pretreated cubic boron nitride powder into toluene according to a solid-to-liquid ratio of 1.2g/L, stirring and dispersing, dropwise adding a coupling agent with the mass of 0.05 times of the cubic boron nitride powder, uniformly dispersing by ultrasonic to obtain a suspension, adding phosphorus oxychloride into the suspension, stirring and reacting for 13 hours at room temperature, adding azodiisobutyronitrile and 1, 1-diphenylethylene, wherein the volume ratio of toluene, phosphorus oxychloride and azoisobutyronitrile is 8:1:0.4, the mass ratio of the cubic boron nitride powder to the 1, 1-diphenylethylene is 1:1.5, introducing argon into an ice salt bath to be pressurized to 0.2MPa, maintaining for 25 minutes, discharging to normal pressure, reacting for 8 hours at the temperature of 60 ℃, filtering after the reaction is finished, washing a filter cake by absolute ethyl alcohol, acetone and deionized water, and drying in vacuum to obtain modified nanometer boron nitride particles.
Preparation of outer sheath pellets
A1: adding 80 parts of polyurethane rubber and 40 parts of ethylene propylene diene monomer rubber into an open mill for plasticating, then adding 15 parts of modified nano boron nitride particles, 6 parts of carbon black and 3 parts of nano zinc oxide, heating to 80 ℃, mixing for 30min, adding 10 parts of methyl silicone oil, 10 parts of flame retardant, 0.5 part of antioxidant and 2 parts of silane coupling agent, heating to 130 ℃, mixing uniformly, and tabletting to obtain master batch;
a2: and (3) placing the masterbatch in an internal mixer, performing triangular package rolling treatment, uniformly mixing, then feeding the masterbatch into a piece, and extruding and granulating the masterbatch at the temperature of 200 ℃ by a double-screw extruder to obtain the outer sheath granules.
Preparation of a Cable
S1: drawing wires of the metal, annealing and twisting to obtain a conductor;
s2: extruding the conductor by an extruding process to obtain an insulating layer;
s3: braiding the outer surface of the insulating layer to obtain a shielding layer;
s4: the shielding layer is externally wrapped by a flame-retardant wrapping tape to obtain an oxygen-isolation flame-retardant layer;
s5: extruding the prepared outer sheath granules on the surface of the oxygen-isolation flame-retardant layer through an extruder, cooling and molding, and irradiating with an irradiation voltage of 1.5MeV and an irradiation current of 20mA at a speed of 200m/min by using a high-energy electron accelerator to obtain a cable finished product.
Example III
Preparation of modified nano boron nitride particles
Adding cubic boron nitride powder into hydrogen peroxide solution, carrying out ultrasonic dispersion, carrying out heat preservation and reflux for 3 hours at the temperature of 60 ℃, filtering, washing a filter cake with deionized water, stirring and dispersing in the deionized water, and carrying out low-temperature plasma treatment by taking air as working gas.
Adding pretreated cubic boron nitride powder into toluene according to the solid-to-liquid ratio of 2g/L, stirring and dispersing, dropwise adding a coupling agent with the mass of 0.05 times of the cubic boron nitride powder, uniformly dispersing by ultrasonic to obtain a suspension, adding phosphorus oxychloride into the suspension, stirring and reacting for 14 hours at room temperature, adding azodiisobutyronitrile and 1, 1-diphenylethylene, wherein the volume ratio of toluene, phosphorus oxychloride and azoisobutyronitrile is 9:1:0.3, the mass ratio of the cubic boron nitride powder to the 1, 1-diphenylethylene is 1:1.5, introducing argon into an ice salt bath to be pressurized to 0.3MPa, maintaining for 30min, discharging to normal pressure, reacting for 8 hours at the temperature of 70 ℃, filtering after the reaction is finished, washing a filter cake with absolute ethyl alcohol, acetone and deionized water, and drying in vacuum to obtain modified nano boron nitride particles.
Preparation of outer sheath pellets
A1: adding 60 parts of polyurethane rubber and 20 parts of ethylene propylene diene monomer rubber into an open mill for plasticating, then adding 25 parts of modified nano boron nitride particles, 4 parts of carbon black and 8 parts of nano zinc oxide, heating to 85 ℃, mixing for 30min, adding 9 parts of methyl silicone oil, 15 parts of flame retardant, 0.4 part of antioxidant and 1 part of silane coupling agent, heating to 140 ℃, mixing uniformly, and tabletting to obtain master batch;
a2: and (3) placing the masterbatch in an internal mixer, performing triangular package rolling treatment, uniformly mixing, then feeding the masterbatch into a piece, and extruding and granulating the masterbatch by a double-screw extruder at the temperature of 175 ℃ to obtain the outer sheath granules.
Preparation of a Cable
S1: drawing wires of the metal, annealing and twisting to obtain a conductor;
s2: extruding the conductor by an extruding process to obtain an insulating layer;
s3: braiding the outer surface of the insulating layer to obtain a shielding layer;
s4: the shielding layer is externally wrapped by a flame-retardant wrapping tape to obtain an oxygen-isolation flame-retardant layer;
s5: extruding the prepared outer sheath granules on the surface of the oxygen-isolation flame-retardant layer through an extruder, cooling and molding, and irradiating with an irradiation voltage of 2MeV, an irradiation current of 40mA and a speed of 300m/min by using a high-energy electron accelerator to obtain a cable finished product.
Comparative example one
This comparative example differs from example one in that the cubic boron nitride powder added to the outer sheath material of this example is a conventional, untreated cubic boron nitride powder.
Comparative example two
The difference between this comparative example and example one is that no modified cubic boron nitride powder was added to the outer sheath material of this comparative example.
The outer sheath materials prepared in the first to third examples and the second example are tableted by a tablet press to obtain test products, and then after the same irradiation crosslinking, the tensile strength, the elongation at break and the heat aging resistance are tested, wherein the aging resistance test is to test the mechanical properties of the test sample after aging after the test sample is subjected to heat preservation at 100 ℃ for 48 hours, and the retention rate of the properties is calculated by comparison with the test sample before aging, and the test results are shown in table 1:
the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the same, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications and equivalents may be made thereto without departing from the spirit and scope of the technical solution of the present invention, which is intended to be covered by the scope of the claims of the present invention. The technology, shape, and construction parts of the present invention, which are not described in detail, are known in the art.
Claims (7)
1. The irradiation crosslinking rubber-based flame-retardant cable comprises a conductor, an insulating layer, a shielding layer, an oxygen-insulating flame-retardant layer and an outer sheath layer from inside to outside, and is characterized in that the outer sheath layer comprises the following raw materials in parts by weight: 60-80 parts of polyurethane rubber, 20-40 parts of ethylene propylene diene monomer rubber, 15-25 parts of modified nano boron nitride particles, 4-6 parts of carbon black, 3-8 parts of nano zinc oxide, 8-10 parts of methyl silicone oil, 10-15 parts of flame retardant, 0.4-0.6 part of antioxidant and 1-2 parts of silane coupling agent; the modified nano boron nitride particles are obtained by grafting and modifying opposite boron nitride by using 1, 1-diphenylethylene; the preparation method of the modified nano boron nitride particles comprises the following steps: adding pretreated cubic boron nitride powder into toluene, stirring and dispersing, dropwise adding a coupling agent, carrying out ultrasonic dispersion to obtain a suspension, adding phosphorus oxychloride into the suspension, stirring at room temperature for reaction for 12-14h, adding azodiisobutyronitrile and 1, 1-diphenylethylene, introducing argon into an ice salt bath for 20-30min, discharging to normal pressure, reacting at 60-80 ℃ for 6-8h at the oil bath temperature, filtering after the reaction is finished, washing a filter cake with absolute ethyl alcohol, acetone and deionized water, and carrying out vacuum drying to obtain modified nano boron nitride particles.
2. The irradiation crosslinking rubber-based flame-retardant cable of claim 1, wherein the outer sheath layer comprises the following raw materials in parts by weight: 75 parts of polyurethane rubber, 30 parts of ethylene propylene diene monomer rubber, 22 parts of modified nano boron nitride particles, 5 parts of carbon black, 6 parts of nano zinc oxide, 8 parts of methyl silicone oil, 12 parts of flame retardant, 0.6 part of antioxidant and 2 parts of silane coupling agent.
3. The irradiation crosslinking rubber-based flame-retardant cable as claimed in claim 2, wherein the pretreatment is to ultrasonically add cubic boron nitride powder into hydrogen peroxide solution, keep the temperature and reflux for 3-4 hours, filter, wash filter cake with deionized water, stir and disperse in deionized water, and perform low-temperature plasma treatment.
4. A method for preparing an irradiation crosslinking rubber-based flame retardant cable according to any of claims 1-3, characterized in that the preparation method specifically comprises the following steps:
s1: drawing wires of the metal, annealing and twisting to obtain a conductor;
s2: extruding the conductor by an extruding process to obtain an insulating layer;
s3: braiding the outer surface of the insulating layer to obtain a shielding layer;
s4: the shielding layer is externally wrapped by a flame-retardant wrapping tape to obtain an oxygen-isolation flame-retardant layer;
s5: and extruding the prepared outer sheath granules on the surface of the oxygen-isolation flame-retardant layer through an extruder, cooling and forming, and irradiating by using a high-energy electron accelerator to obtain a cable finished product.
5. The method for preparing the irradiation crosslinking rubber-based flame-retardant cable as claimed in claim 4, wherein the irradiation parameters of the high-energy electron accelerator are as follows: the irradiation voltage is 1.5-2MeV, the irradiation current is 20-60mA, and the speed is 200-400m/min.
6. The method for preparing the irradiation crosslinking rubber-based flame-retardant cable according to claim 5, wherein the preparation method of the outer sheath granule is as follows:
a1: adding polyurethane rubber and ethylene propylene diene monomer into an open mill for plasticating, then adding modified nano boron nitride particles, carbon black and nano zinc oxide, heating to 80-90 ℃, mixing for 30min, adding methyl silicone oil, a flame retardant, an antioxidant and a silane coupling agent, heating to 120-140 ℃, mixing uniformly, and tabletting for molding to obtain master batch;
a2: placing the masterbatch in an internal mixer, performing triangular package rolling treatment, uniformly mixing, then discharging, and extruding and granulating by a double-screw extruder to obtain the outer sheath granules.
7. The method for preparing an irradiation crosslinking rubber-based flame retardant cable as claimed in claim 6, wherein the temperature of the twin screw extruder is 175-220 ℃.
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