CN112225983A - Flame-retardant sheath material for nuclear power station cable, preparation method and service life detection method - Google Patents
Flame-retardant sheath material for nuclear power station cable, preparation method and service life detection method Download PDFInfo
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Abstract
The invention discloses a flame-retardant sheath material for a nuclear power station cable, which comprises a polymer base material and a radiation grafting compatilizer: an inorganic flame retardant; zinc borate; an organic flame retardant hexaphenoxycyclotriphosphazene; ammonium octamolybdate as a smoke suppressant; anti-aging agent RD (2, 2, 4-trimethyl-1, 2-dihydroquinoline polymer); compounding antioxidant; an anti-radiation agent; a lubricant; the polymer base material comprises an ethylene-vinyl acetate copolymer, an ethylene-ethyl acrylate copolymer and an ethylene-methyl methacrylate copolymer; the radiation grafting compatilizer comprises ethylene-vinyl acetate copolymer of radiation grafting maleic anhydride and/or linear low-density polyethylene of radiation grafting maleic anhydride and/or ethylene-octene copolymer of radiation grafting maleic anhydride. The cable sheath layer of the nuclear power station meets the requirement of 60-year service life of third-generation nuclear power, has high irradiation resistance and can burn class A/B by bundling.
Description
Technical Field
The invention relates to the technical field of cables, in particular to a flame-retardant sheath material for a nuclear power station cable, a preparation method and a service life detection method.
Background
Nuclear power is a safe, clean and economical energy source. The long-term service life of the nuclear reactor type of the third generation, such as AP1000, CAP1400, Hualong I and the like, is improved to 60 years at 90 ℃ on the basis of 40 years of long-term service life of the nuclear reactor type of the second generation at 90 ℃. The nuclear power 1E-level cable used in the nuclear power station has very harsh working environment, and in the whole life span, the cable must withstand the comprehensive effect of intersection of multiple factors such as an electric field, temperature, oxygen, nuclear radiation, steam, moisture, chemicals and the like under the nuclear environment condition.
A halogen-free flame retardant system is adopted for cable sheath materials for nuclear power stations, a large amount of inorganic flame retardant is required to be added for flame retarding of finished cables through bundling combustion of A/B type, the mechanical property of the cable materials is reduced, in order to improve the mechanical property of the materials, a chemical grafting compatilizer is usually added in a formula to improve the compatibility of the inorganic flame retardant and a polymer base material, and a radiation grafting compatilizer has certain gel content (less than or equal to 10%) after irradiation of an electron accelerator besides maleic anhydride groups with improved compatibility, so that the mechanical property of the compatilizer is improved, the mechanical property of the sheath materials is also improved, and meanwhile, the gel content is lower, and the processing property of the materials is not influenced.
In addition, the cable sheath material for the conventional nuclear power station adopts a radiation crosslinking formula, such as a halogen-free flame-retardant sheath material in a nuclear island disclosed in Chinese patent (CN109575409A), and the specific formula is as follows: polymer base material: 100 parts of (A); inorganic flame retardant: 80-100 parts of a binder; zinc borate: 15-25 parts; polyphosphazene flame retardant: 8-12 parts; phosphorus-nitrogen flame retardant: 8-12 parts; ammonium octamolybdate as smoke agent: 1-3 parts; anti-aging agent RD (2, 2, 4-trimethyl-1, 2-dihydroquinoline polymer): 1-3 parts; compound antioxidant: 4-8 parts; an anti-irradiation agent: 3-8 parts; processing aid: 6-12 parts; wherein the processing aid comprises a crosslinking sensitizer and a lubricant. The sheath material has excellent performance, good flame retardant property, stable irradiation resistance, electrical property and mechanical property, low smoke, no halogen and low toxicity, and has the three-generation nuclear power service life of 60 years and the resistance of 2400kGy gamma rays.
The nuclear power cable sheath layer prepared by adopting the radiation crosslinking halogen-free flame-retardant sheath material for the nuclear power station has excellent performance, but an electron accelerator is required to be adopted for radiation crosslinking, so that the process has the defects of complex process and high cost.
Disclosure of Invention
The invention aims to provide a flame-retardant sheath material for a nuclear power station cable, a preparation method and a life detection method, wherein the nuclear power station cable sheath layer prepared by the material has the service life of 60 years of third-generation nuclear power, has high radiation resistance (gamma ray is more than or equal to 2000kGy), is subjected to A/B class through bundling combustion, and is low in smoke, halogen and toxicity.
The flame-retardant sheath material for the nuclear power station cable comprises the following raw materials in parts by weight:
polymeric substrate and radiation graft compatibilizer: 95-105 parts; inorganic flame retardant: 80-100 parts of a binder; zinc borate: 15-25 parts; organic flame retardant hexaphenoxycyclotriphosphazene: 8-12 parts; ammonium octamolybdate as smoke agent: 1-3 parts; anti-aging agent RD (2, 2, 4-trimethyl-1, 2-dihydroquinoline polymer): 1-3 parts; compound antioxidant: 4-8 parts; an anti-irradiation agent: 3-8 parts; lubricant: 3-5 parts;
wherein the polymer substrate comprises an ethylene-vinyl acetate copolymer, an ethylene-ethyl acrylate copolymer and an ethylene-methyl methacrylate copolymer;
the radiation grafting compatilizer comprises ethylene-vinyl acetate copolymer of radiation grafting maleic anhydride and/or linear low-density polyethylene of radiation grafting maleic anhydride and/or ethylene-octene copolymer of radiation grafting maleic anhydride;
the composite antioxidant comprises a main antioxidant, an auxiliary antioxidant and an ultraviolet absorbent, wherein:
the main antioxidant comprises pentaerythritol tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ] and/or octadecyl beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate and/or N, N' -bis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl ] hydrazine;
the auxiliary antioxidant comprises thioester antioxidant of didodecyl thiodipropionate (DLTP) and/or dioctadecyl thiodipropionate (DSTP);
the ultraviolet absorbent comprises 2- (2 '-hydroxy-3', 5 '-ditert-amyl-phenyl) benzotriazole and/or 2- (2' -hydroxy-5 '-tert-octyl-phenyl) benzotriazole and/or 2- (2' -hydroxy-3 ',5' -bis (a, a-dimethylbenzyl) phenyl) benzotriazole;
the anti-irradiation agent comprises an anti-irradiation agent A and an anti-irradiation agent B, wherein the anti-irradiation agent A is high phenyl silicone rubber and/or phenylene silicone rubber, and the anti-irradiation agent B is boron carbide and/or boron nitride;
the lubricant comprises one or more of polyethylene wax, zinc stearate, calcium stearate, ethylene bis stearamide, EBS, and silicone masterbatch.
A preparation method of a flame-retardant sheath material of a nuclear power station cable comprises the steps of putting a polymer base material, a radiation grafting compatilizer, magnesium hydroxide and aluminum hydroxide in an inorganic flame retardant, zinc borate, an organic flame retardant hexaphenoxycyclotriphosphazene, a smoke agent ammonium octamolybdate, an anti-aging agent RD (2, 2, 4-trimethyl-1, 2-dihydroquinoline polymer), a composite antioxidant, an anti-irradiation agent B and a lubricant into an internal mixer for mixing, melting, mixing for 4-6 minutes at the temperature of 125-plus 135 ℃, adding the anti-irradiation agent A, mixing for 5-10 minutes at the temperature of 130-plus 150 ℃, lifting to a double-stage extruder, and carrying out air-cooled extrusion granulation at the temperature of 120-plus 160 ℃.
The pellets prepared in claim 8 are melt extruded at a temperature of 120-160 ℃ in a single screw extruder to form a thermoplastic halogen-free flame retardant sheath for a cable in a nuclear power plant.
The thermal life test of the nuclear power thermoplastic halogen-free flame-retardant sheath material is carried out according to the GB/T1040.3-2006 specification, the test sample is a 5-type dumbbell piece, the thickness is 2.0 +/-0.2 mm, a natural ventilation electric heating ageing oven is adopted, the replacement frequency of air in the ageing oven per hour is 8-20 times, the test temperatures are 180 +/-2 ℃ and 165 +/-2 ℃ respectively, the test sample is placed on a stainless steel flat plate with talcum powder spread in an ageing oven, the test temperatures are 150 +/-2 ℃ and 135 +/-2 ℃ respectively, the test sample is vertically hung in an effective working area in the middle of the ageing oven, and after ageing at 4 temperature points, the service life of the three-generation nuclear power thermoplastic halogen-free flame-retardant sheath material is deduced according to the Arrhenius formula.
The invention has the advantages that: the invention adopts the halogen-free flame-retardant sheath material for the thermoplastic nuclear power station to replace a radiation crosslinking material, meets the requirement of the third-generation nuclear power for 60-year service life (the environmental temperature of 90 ℃), has the cable sheath layer with the A/B type through bundling combustion, has low smoke, no halogen, low toxicity and high radiation resistance (gamma ray is more than or equal to 2000kGy), can be applied to the cable sheath layers in the third-generation nuclear power island (K1) and outside the island (K2 and K3), simplifies the production process of the cable for the nuclear power station, reduces the production cost and expands the variety of the nuclear power cable, and has great significance.
Detailed Description
For the convenience of description in the examples that follow, the following substances are set for short, in particular as follows:
for short, ethylene-vinyl acetate copolymers: EVA;
for short, ethylene-ethyl acrylate copolymer: EEA;
the ethylene-methyl methacrylate copolymer is abbreviated as: EMMA
The ethylene-vinyl acetate copolymer of radiation grafted maleic anhydride is abbreviated as: EVA-g-MAH
The linear low density polyethylene radiation grafted with maleic anhydride is abbreviated as: LLDPE-g-MAH;
the ethylene-octene copolymer of radiation grafted maleic anhydride is abbreviated: POE-g-MAH;
for short, linear low density polyethylene: LLDPE;
the ethylene-octene copolymer is abbreviated as: POE;
the main antioxidant comprises pentaerythritol tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate, which is simply referred to as: 1010;
octadecyl beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate: 300, respectively;
the abbreviation of N, N' -bis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl ] hydrazine: 1024;
the thioester antioxidant, didodecyl thiodipropionate, is abbreviated as: DLTP;
dioctadecyl thiodipropionate abbreviated as: DSTP;
2- (2' -hydroxy-3 ',5' -ditert-pentylphenyl) benzotriazole: UV 328;
for 2- (2 '-hydroxy-5' -tert-octylphenyl) benzotriazole: UL 328;
2- (2' -hydroxy-3 ',5' -bis (a, a-dimethylbenzyl) phenyl) benzotriazole: UL 234.
The present invention is described in detail below:
the flame-retardant sheath material for the nuclear power station cable comprises the following raw materials in parts by weight:
polymeric substrate and radiation graft compatibilizer: 95-105 parts; inorganic flame retardant: 80-100 parts of a binder; zinc borate: 15-25 parts; organic flame retardant hexaphenoxycyclotriphosphazene: 8-12 parts; ammonium octamolybdate as smoke agent: 1-3 parts; anti-aging agent RD (2, 2, 4-trimethyl-1, 2-dihydroquinoline polymer): 1-3 parts; compound antioxidant: 4-8 parts; an anti-irradiation agent: 3-8 parts; lubricant: 3-5 parts.
Wherein the polymer substrate comprises ethylene-vinyl acetate copolymer (EVA), ethylene-ethyl acrylate copolymer (EEA) and ethylene-methyl methacrylate copolymer (EMMA), and the amount of vinyl acetate, ethyl acrylate and methyl methacrylate in the ethylene-vinyl acetate copolymer (EVA), the ethylene-ethyl acrylate copolymer (EEA) and the ethylene-methyl methacrylate copolymer (EMMA) is 14-40% of the total amount of the polymer substrate;
the melt index MI of ethylene-vinyl acetate copolymer (EVA), ethylene-ethyl acrylate copolymer (EEA) and ethylene-methyl methacrylate copolymer (EMMA) is 2-6.
The radiation grafting compatilizer comprises ethylene-vinyl acetate copolymer (EVA-g-MAH) of radiation grafted maleic anhydride and/or linear low density polyethylene (LLDPE-g-MAH) of radiation grafted maleic anhydride and/or ethylene-octene copolymer (POE-g-MAH) of radiation grafted maleic anhydride.
The radiation grafting compatilizer is prepared by the following method: dissolving 1-5 parts of maleic anhydride in 10 parts of acetone, mixing 0.1-0.5 part of main antioxidant and 95-105 parts of ethylene-vinyl acetate copolymer (EVA) or 95-105 parts of Linear Low Density Polyethylene (LLDPE) or 100 parts of ethylene-octene copolymer (POE) in a high-speed mixer at the temperature of 30-50 ℃ for 5-15 minutes, extruding water-cooling strand-drawing and grain-cutting in a double-screw extruder at the temperature of 100 ℃ after the acetone is completely volatilized to obtain ungrafted master batches, placing the ungrafted master batches on a radiation trolley flat plate under a 3-5M electron accelerator, wherein the thickness of the ungrafted master batches is not more than 2cm, the radiation dose is 10-25kGy, and preparing the radiation grafting compatilizer with the grafting rate of 1-3% and the gel content of not more than 10%.
The weight portion ratio of ethylene-vinyl acetate copolymer (EVA-g-MAH) of radiation grafting maleic anhydride, linear low-density polyethylene (LLDPE-g-MAH) of radiation grafting maleic anhydride, ethylene-octene copolymer (POE-g-MAH) of radiation grafting maleic anhydride, ethylene-vinyl acetate copolymer (EVA), ethylene-ethyl acrylate copolymer (EEA) and ethylene-methyl methacrylate copolymer (EMMA) is 0-5: 5-10: 0-5: 0-20: 20-50: 10-30.
The inorganic flame retardant comprises magnesium hydroxide and aluminum hydroxide, wherein the weight part ratio of the magnesium hydroxide to the aluminum hydroxide is (40-60): 20-40.
The composite antioxidant comprises a main antioxidant, an auxiliary antioxidant and an ultraviolet absorbent, wherein:
the main antioxidant comprises pentaerythritol tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ] (1010) and/or octadecyl beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate (300) and/or N, N' -bis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl ] hydrazine (1024).
The auxiliary antioxidant comprises thioester antioxidant of didodecyl thiodipropionate (DLTP) and/or dioctadecyl thiodipropionate (DSTP).
The ultraviolet absorbent comprises 2- (2 '-hydroxy-3', 5 '-ditert-amyl-phenyl) benzotriazole (UV328) and/or 2- (2' -hydroxy-5 '-tert-octyl-phenyl) benzotriazole (UL328) and/or 2- (2' -hydroxy-3 ',5' -bis (a, a-dimethylbenzyl) phenyl) benzotriazole (UL 234).
The weight part ratio of the pentaerythritol tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ] (1010), the octadecyl beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate (300) and the N, N' -bis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl ] hydrazine (1024) is 1: 0.5-1.5: 0.5-1.5.
The anti-irradiation agent comprises an anti-irradiation agent A and an anti-irradiation agent B, wherein the anti-irradiation agent A is high phenyl silicone rubber and/or phenylene silicone rubber, and the anti-irradiation agent B is boron carbide and/or boron nitride; the weight part ratio of the high phenyl silicone rubber and the phenylene silicone rubber in the anti-irradiation agent A is 8-12: 0-2, wherein the weight part ratio of boron carbide to boron nitride in the anti-radiation agent B is 1-2: 1-2.
The lubricant comprises one or more of polyethylene wax, zinc stearate, calcium stearate, ethylene bis stearamide, EBS, and silicone masterbatch.
A preparation method of a flame-retardant sheath material of a nuclear power station cable comprises the steps of putting a polymer base material, magnesium hydroxide and aluminum hydroxide in an inorganic flame retardant, zinc borate, an organic flame retardant hexaphenoxycyclotriphosphazene, a smoke agent ammonium octamolybdate, an anti-aging agent RD (2, 2, 4-trimethyl-1, 2-dihydroquinoline polymer), a composite antioxidant, an anti-irradiation agent B and a lubricant into an internal mixer for mixing, mixing for 4-6 minutes after melting to 125-135 ℃, then adding the anti-irradiation agent A, mixing for 5-10 minutes within the temperature range of 130-150 ℃, lifting to a double-stage double-screw extruder, and carrying out air cooling extrusion granulation within the temperature range of 120-160 ℃.
The prepared particles are melted and extruded at the temperature of 120-160 ℃ in a single-screw extruder to form the thermoplastic halogen-free flame-retardant sheath of the cable of the nuclear power station.
According to the method for testing the service life of the prepared sheath, a thermal life test of the nuclear power thermoplastic halogen-free flame-retardant sheath material is carried out according to GB/T1040.3-2006, the test sample is a 5-type dumbbell sheet, the thickness is 2.0 +/-0.2 mm, a natural ventilation electric heating ageing oven is adopted, the number of times of air replacement in the ageing oven per hour is 8-20, the test temperatures are 180 +/-2 ℃ and 165 +/-2 ℃, the test sample is placed on a stainless steel flat plate with talcum powder spread in the ageing oven, the test temperatures are 150 +/-2 ℃ and 135 +/-2 ℃, the test sample is vertically hung in an effective working area in the middle of the ageing oven, and after ageing at 4 temperature points, the service life of the three-generation nuclear power thermoplastic halogen-free flame-retardant sheath material is deduced according to Arenrhaus equation.
The invention is further illustrated by the following examples.
The method comprises the following operation steps:
dissolving 3 parts of maleic anhydride in 10 parts of acetone, mixing the maleic anhydride with 0-0.5 part of main antioxidant 1010 and 95 parts of ethylene-vinyl acetate copolymer in a high-speed mixer at the temperature of 30-50 ℃ for 5-15 minutes, extruding out water-cooled drawing strips and cutting granules in a double-screw extruder at the temperature of 100 ℃ and 150 ℃ after the acetone is completely volatilized to obtain ungrafted master batches, placing the ungrafted master batches on an irradiation trolley flat plate under a 3-5M electronic accelerator, wherein the thickness of the ungrafted master batches is not more than 2cm (too thick, the accelerator cannot completely penetrate the ungrafted master batches), and the irradiation dose is 20kGy to obtain the radiation grafting compatilizer with the grafting rate of 1-3% and the gel content of less than or equal to 10%.
EXAMPLES 1 to 3 Performance test
| Test items | Case 1 | Case 2 | Case 3 |
| 1. Tensile Strength (MPa) | 12.8 | 13.3 | 13.8 |
| 2. Elongation at Break (%) | 680.34 | 709.12 | 725.11 |
| 3. Graft ratio (%) | 1.25 | 1.21 | 1.18 |
| 4. Gel content (%) | 8.86 | 8.09 | 7.87 |
The comparison of the ethylene-vinyl acetate copolymer of radiation grafted maleic anhydride prepared in cases 1-3 of the present invention with the properties of the EVA material shows that the EVA material has the lowest strength and the highest elongation, while the EVA material grafted by radiation has the highest strength and the lowest elongation due to radiation grafting, and meanwhile, the molecular bond of the polymer is partially broken under the action of high shear of the EVA material heated in a twin-screw extruder, and if no antioxidant material is added, the breaking degree of the molecular bond is significantly greater than that of the antioxidant material, which is mainly reflected in the mechanical properties of the material.
The invention is further illustrated by the following specific examples.
Example 1
Raw materials:
the method comprises the following operation steps:
radiation grafting compatilizers EVA-g-MAH, LLDPE-g-MAH, polymer base material: EVA, EEA, EMMA, antioxidant RD2, 2, 4-trimethyl-1, 2-dihydroquinoline polymer), primary antioxidant: 1010. 1024, secondary antioxidant: DLTP, ultraviolet absorber: placing UV328, zinc stearate, ethylene bis stearamide EBS, silicone master batch, ammonium octamolybdate, boron carbide, magnesium hydroxide, aluminum hydroxide, zinc borate, hexaphenoxycyclotriphosphazene and environment-friendly black master batch into a 75-liter internal mixer, mixing for 6 minutes at 125 ℃ after melting, then adding an anti-irradiation agent of high phenyl silicone rubber (the phenyl content is 40%) and phenylene silicone rubber (the phenylene content is 60%), mixing for 10 minutes at 130 ℃, then lifting to a double-stage double-screw extruder, and carrying out air-cooling extrusion granulation at 150 ℃ to obtain the product;
example 2
Raw materials:
the method comprises the following operation steps:
radiation grafting of a compatibilizer: EVA-g-MAH, POE-g-MAH, polymer substrate: EVA, EEA, EMMA, antioxidant RD (2, 2, 4-trimethyl-1, 2-dihydroquinoline polymer), antioxidant: 1010. 1024, secondary antioxidant: DLTP, ultraviolet absorber: placing UV328, zinc stearate, Ethylene Bis Stearamide (EBS), silicone master batch, ammonium octamolybdate, boron carbide, magnesium hydroxide, aluminum hydroxide, zinc borate, hexaphenoxycyclotriphosphazene and environment-friendly black master batch into a 75-liter internal mixer, mixing for 5.5 minutes after melting to about 128 ℃, then adding an anti-irradiation agent high phenyl silicone rubber (with the phenyl content of 40%) and phenylene silicone rubber (with the phenylene content of 60%), mixing for 9 minutes at 135 ℃, then lifting to a double-stage double-screw extruder, and carrying out air-cooling extrusion granulation at 155 ℃ to obtain the product;
example 3
Raw materials:
the method comprises the following operation steps:
radiation grafting compatilizer polymers EVA-g-MAH and POE-g-MAH, and a polymer substrate: EVA, EEA, EMMA, antioxidant RD (2, 2, 4-trimethyl-1, 2-dihydroquinoline polymer), primary antioxidant: 1010. 1024, secondary antioxidant: DLTP, ultraviolet absorber: placing UV328, zinc stearate, Ethylene Bis Stearamide (EBS), silicone master batch, ammonium octamolybdate, boron carbide, magnesium hydroxide, aluminum hydroxide, zinc borate, hexaphenoxycyclotriphosphazene and environment-friendly black master batch into a 75-liter internal mixer, mixing for 5 minutes at 130 ℃ after melting, then adding an anti-irradiation agent high phenyl silicone rubber (with the phenyl content of 40%), mixing for 8 minutes at 138 ℃, then lifting to a double-stage double-screw extruder, and performing air-cooled extrusion granulation at 145 ℃ to obtain the high-performance silicon rubber;
example 4
Raw materials:
the method comprises the following operation steps:
radiation grafting of a compatibilizer: EVA-g-MAH, POE-g-MAH, LLDPE-g-MAH, polymer base material: EVA, EEA, EMMA, antioxidant RD (2, 2, 4-trimethyl-1, 2-dihydroquinoline polymer), primary antioxidant 1010, 1024, secondary antioxidant: DLTP, ultraviolet absorber: placing UV328, zinc stearate, Ethylene Bis Stearamide (EBS), silicone master batch, ammonium octamolybdate, boron carbide, magnesium hydroxide, aluminum hydroxide, zinc borate, hexaphenoxycyclotriphosphazene and environment-friendly black master batch into a 75-liter internal mixer, mixing for 4.8 minutes at 132 ℃ after melting, then adding an anti-irradiation agent high phenyl silicone rubber (with the phenyl content of 40%), mixing for 7 minutes at 140 ℃, lifting to a double-stage double-screw extruder, and carrying out air-cooled extrusion granulation at 140 ℃ to obtain the high-performance silicon rubber;
example 5
Raw materials:
the method comprises the following operation steps:
radiation grafting of a compatibilizer: POE-g-MAH, EVA-g-MAH, polymer substrate: EVA, EEA, EMMA, antioxidant RD (2, 2, 4-trimethyl-1, 2-dihydroquinoline polymer), primary antioxidant: 1010. 1024, secondary antioxidant: DLTP, ultraviolet absorber: placing UV328, zinc stearate, Ethylene Bis Stearamide (EBS), silicone master batch, ammonium octamolybdate, boron carbide, magnesium hydroxide, aluminum hydroxide, zinc borate, hexaphenoxycyclotriphosphazene and environment-friendly black master batch into a 75-liter internal mixer, mixing for 4.5 minutes after melting to about 134 ℃, then adding an anti-irradiation agent high phenyl silicone rubber (with the phenyl content of 40%), mixing for 6 minutes at the temperature of 144 ℃, lifting to a double-stage double-screw extruder, and carrying out air-cooled extrusion granulation at the temperature of 135 ℃ to obtain the high phenyl silicone rubber;
example 6
Raw materials:
the method comprises the following operation steps:
radiation grafting of a compatibilizer: POE-g-MAH, EVA-g-MAH, polymer substrate: EVA, EEA, EMMA, antioxidant RD (2, 2, 4-trimethyl-1, 2-dihydroquinoline polymer), primary antioxidant 1010, 1024, secondary antioxidant: DLTP, ultraviolet absorber: placing UV328, zinc stearate, Ethylene Bis Stearamide (EBS), silicone master batch, ammonium octamolybdate, boron carbide, magnesium hydroxide, aluminum hydroxide, zinc borate, hexaphenoxycyclotriphosphazene and environment-friendly black master batch into a 75-liter internal mixer, mixing for 4.3 minutes after melting to about 134 ℃, then adding an anti-irradiation agent high phenyl silicone rubber (with the phenyl content of 40%), mixing for 6 minutes at 147 ℃, then lifting to a double-stage double-screw extruder, and carrying out air-cooled extrusion granulation at 130 ℃ to obtain the high phenyl silicone rubber;
example 7
Raw materials:
radiation grafting of a compatibilizer: POE-g-MAH, EVA-g-MAH, polymer: EVA, EEA, EMMA, antioxidant RD (2, 2, 4-trimethyl-1, 2-dihydroquinoline polymer), primary antioxidant: 1010. 1024, secondary antioxidant: DLTP, ultraviolet absorber: placing UV328, zinc stearate, Ethylene Bis Stearamide (EBS), silicone master batch, ammonium octamolybdate, boron carbide, magnesium hydroxide, aluminum hydroxide, zinc borate, hexaphenoxycyclotriphosphazene and environment-friendly black master batch into a 75-liter internal mixer, mixing for 4 minutes after melting to about 135 ℃, then adding an anti-irradiation agent high phenyl silicone rubber (with the phenyl content of 40%), mixing for 5 minutes at the temperature of 150 ℃, then lifting to a double-stage double-screw extruder, and carrying out air-cooling extrusion granulation at the temperature of 125 ℃ to obtain the high phenyl silicone rubber;
application examples
The particle material of the third-generation nuclear power thermoplastic halogen-free flame-retardant sheath of the embodiments 1-7 is melted and extruded at the temperature of 120-160 ℃ of a phi 45-120 single-screw extruder according to the GB/T12706.1-2008 cable manufacturing method to form the thermoplastic halogen-free flame-retardant sheath of the nuclear power plant cable, the sheath is coated on the radiation cross-linked double-layer insulating core wire and/or the coated halogen-free flame-retardant filling layer (oxygen-isolating layer) cable, and the thickness of the sheath can be determined according to various cable specification requirements.
The third-generation nuclear power thermoplastic halogen-free flame-retardant sheath material and the cable prepared from the same have the performance shown in the table.
Table 1: test methods and standards of each test item:
TABLE 2 thermoplastic halogen-free flame-retardant sheathing compound and cable property
Table 2 (continuation)
By comparing the performance of the third-generation nuclear power thermoplastic halogen-free flame-retardant sheath material prepared in the embodiments 1-7 of the invention and the nuclear power cable prepared from the same, the following results can be obtained:
(1) the formulations of example 1 and example 2 are adopted, the POE-g-MAH in example 2 replaces the LLDPE-g-MAH in example 1, the other formulation components are kept consistent, the tensile strength of example 2 is slightly lower than that of example 1, the elongation at break is slightly higher, the other properties are basically kept consistent, and POE belongs to polyolefin elastomer, the tensile strength of POE is lower than that of LLDPE, and the elongation at break is higher.
(2) The formulations of the embodiment 2 and the embodiment 3 are adopted, the content of phenylene in the radiation resistant agent phenylene silicone rubber (the content of phenylene in the silicone rubber is 60%) is reduced in the embodiment 3, the components of the other formulations are kept consistent, and the radiation resistance of the embodiment 3 is obviously reduced compared with that of the embodiment 2, which shows that the phenylene silicone rubber (the content of phenylene in the silicone rubber is 60%) has excellent radiation resistance, but the cost is high, and the raw materials are not easy to purchase.
(3) The formulations of example 3 and example 4, example 4 adopted three compatilizers, the weight is 7.5kg, the weight of EMMA is 22.5kg, example 3 adopted two compatilizers, the weight is 5kg, the weight of EMMA is 25kg, other formulation components are kept consistent, the performance of example 4 is improved, the strength is improved, the elongation is reduced, the aging performance is slightly reduced, the material strength can be improved by increasing the types and the weights of the compatilizers, but the elongation is reduced at the same time, and the EMMA heat resistance is better than that of the compatilizers.
(4) The formulations of the embodiment 5 and the embodiment 3 are that the inorganic flame retardants magnesium hydroxide and aluminum hydroxide are exchanged by weight, the elongation at break of the embodiment 5 is obviously improved compared with that of the embodiment 3, the aging performance is slightly lower, the flame retardant performance is obviously reduced, the small-sized cable is unqualified in flame retardant, the aluminum hydroxide is obviously inferior to the magnesium hydroxide in flame retardant performance, the heat resistance is slightly inferior, but the compatibility with the polymer is much better than that of the magnesium hydroxide.
(5) The formulations of examples 6 and 3 are shown, wherein 10kg of zinc borate and 3kg of hexaphenoxycyclotriphosphazene are used in example 6, 8kg of zinc borate and 5kg of hexaphenoxycyclotriphosphazene are used in example 3, the flame retardance of the cable with small specification is obviously reduced, but the smoke density of the material is better, and the flame retardance of the hexaphenoxycyclotriphosphazene is obviously better than that of the zinc borate, but the smoke density is higher.
(6) The formulations of example 7 and example 6 are shown, wherein the zinc borate is 5kg, the hexaphenoxy cyclotriphosphazene is 8kg in example 7, the zinc borate is 10kg in example 6, and the hexaphenoxy cyclotriphosphazene is 3kg, and the material of example 7 has good flame retardant property, but the smoke density is obviously increased, and the smoke density of a large-specification cable is unqualified. The obtained hexaphenoxycyclotriphosphazene has good flame retardance but high smoke density, and the dosage is controlled when the hexaphenoxycyclotriphosphazene is used.
Claims (10)
1. The flame-retardant sheath material for the nuclear power station cable is characterized by comprising the following raw materials in parts by weight:
polymeric substrate and radiation graft compatibilizer: 95-105 parts; inorganic flame retardant: 80-100 parts of a binder; zinc borate: 15-25 parts; organic flame retardant hexaphenoxycyclotriphosphazene: 8-12 parts; ammonium octamolybdate as smoke agent: 1-3 parts; anti-aging agent RD (2, 2, 4-trimethyl-1, 2-dihydroquinoline polymer): 1-3 parts; compound antioxidant: 4-8 parts; an anti-irradiation agent: 3-8 parts; lubricant: 3-5 parts;
wherein the polymer substrate comprises an ethylene-vinyl acetate copolymer, an ethylene-ethyl acrylate copolymer and an ethylene-methyl methacrylate copolymer;
the radiation grafting compatilizer comprises ethylene-vinyl acetate copolymer of radiation grafting maleic anhydride and/or linear low-density polyethylene of radiation grafting maleic anhydride and/or ethylene-octene copolymer of radiation grafting maleic anhydride;
the composite antioxidant comprises a main antioxidant, an auxiliary antioxidant and an ultraviolet absorbent, wherein:
the main antioxidant comprises pentaerythritol tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ] and/or octadecyl beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate and/or N, N' -bis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl ] hydrazine;
the auxiliary antioxidant comprises thioester antioxidant of didodecyl thiodipropionate (DLTP) and/or dioctadecyl thiodipropionate (DSTP);
the ultraviolet absorbent comprises 2- (2 '-hydroxy-3', 5 '-ditert-amyl-phenyl) benzotriazole and/or 2- (2' -hydroxy-5 '-tert-octyl-phenyl) benzotriazole and/or 2- (2' -hydroxy-3 ',5' -bis (a, a-dimethylbenzyl) phenyl) benzotriazole;
the anti-irradiation agent comprises an anti-irradiation agent A and an anti-irradiation agent B, wherein the anti-irradiation agent A is high phenyl silicone rubber and/or phenylene silicone rubber, and the anti-irradiation agent B is boron carbide and/or boron nitride;
the lubricant comprises one or more of polyethylene wax, zinc stearate, calcium stearate, ethylene bis stearamide, EBS, and silicone masterbatch.
2. The flame-retardant sheath material for the nuclear power plant cable according to claim 1, wherein the radiation grafting compatilizer is prepared by the following method: dissolving 1-5 parts of maleic anhydride in 10 parts of acetone, mixing with 0-0.5 part of main antioxidant and 95-105 parts of ethylene-vinyl acetate copolymer or 95-105 parts of linear low-density polyethylene or 100 parts of ethylene-octene copolymer in a high-speed mixer at the temperature of 30-50 ℃ for 5-15 minutes, extruding out water-cooling ribbing and grain-cutting in a double-screw extruder at the temperature of 100 ℃ and 150 ℃ after the acetone is completely volatilized to obtain ungrafted master batches, placing the ungrafted master batches on an irradiation trolley flat plate under a 3-5M electron accelerator, wherein the thickness of the ungrafted master batches is not more than 2cm, the irradiation dose is 10-25kGy, and preparing the radiation grafting compatilizer with the grafting rate of 1-3 percent and the gel content of less than or equal to 10 percent.
3. The flame-retardant sheath material for the cable of the nuclear power station as claimed in claim 1, wherein the weight ratio of the radiation grafted maleic anhydride ethylene-vinyl acetate copolymer, the radiation grafted maleic anhydride linear low density polyethylene, the radiation grafted maleic anhydride ethylene-octene copolymer, the ethylene-vinyl acetate copolymer, the ethylene-ethyl acrylate copolymer and the ethylene-methyl methacrylate copolymer is 0-5: 5-10: 0-5: 0-20: 20-50: 10-30.
4. The flame-retardant sheath material for the nuclear power plant cable according to claim 1, wherein the flame-retardant sheath material comprises an ethylene-vinyl acetate copolymer, an ethylene-ethyl acrylate copolymer and an ethylene-methyl methacrylate copolymer, wherein the weight ratio of the ethylene-vinyl acetate copolymer to the ethylene-ethyl acrylate copolymer is as follows: the amount of vinyl acetate, ethyl acrylate and methyl methacrylate is 14-40% of the total amount of the polymer base material;
the melt index MI of the ethylene-vinyl acetate copolymer, the ethylene-ethyl acrylate copolymer and the ethylene-methyl methacrylate copolymer is 2-6.
5. The flame-retardant sheath material for the nuclear power plant cable according to claim 1, wherein the inorganic flame retardant comprises magnesium hydroxide and aluminum hydroxide, and the weight part ratio of the magnesium hydroxide to the aluminum hydroxide is 40-60: 20-40.
6. The flame-retardant sheath material for the cable in the nuclear power plant as claimed in claim 1, wherein the weight part ratio of the pentaerythritol tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], the octadecyl beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate and the N, N' -bis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl ] hydrazine is 1: 0.5-1.5: 0.5-1.5.
7. The flame-retardant sheath material for the nuclear power station cable according to claim 1, wherein the radiation-resistant agent A comprises 8-12 parts by weight of high phenyl silicone rubber and phenylene silicone rubber: 0-2, wherein the weight part ratio of boron carbide to boron nitride in the anti-radiation agent B is 1-2: 1-2.
8. The method for preparing the flame-retardant sheath material of the nuclear power plant cable according to any one of claims 1 to 6, wherein: the polymer base material, the radiation grafting compatilizer, magnesium hydroxide and aluminum hydroxide in the inorganic flame retardant, zinc borate, the organic flame retardant hexaphenoxycyclotriphosphazene, the smoke suppressor ammonium octamolybdate, the anti-aging agent RD (2, 2, 4-trimethyl-1, 2-dihydroquinoline polymer), the composite antioxidant, the anti-irradiation agent B and the lubricant are put into an internal mixer for mixing, the mixture is melted and mixed for 4 to 6 minutes at the temperature of 125 plus materials and 135 ℃, then the anti-irradiation agent A is added, the mixture is mixed for 5 to 10 minutes at the temperature of 130 plus materials and 150 ℃, and then the mixture is lifted to a double-stage double-screw extruder, and the mixture is extruded and granulated at the temperature of 120 plus materials and 160 ℃.
9. The nuclear power thermoplastic halogen-free flame-retardant sheath of the nuclear power station cable is characterized in that: the pellets prepared in claim 8 are melt extruded at a temperature of 120-160 ℃ in a single screw extruder to form a thermoplastic halogen-free flame retardant sheath for a cable in a nuclear power plant.
10. A method for testing the service life of the sheath prepared according to claim 9 is characterized in that a thermal life test of the nuclear power thermoplastic halogen-free flame-retardant sheath material is carried out according to GB/T1040.3-2006, the sample is a 5-type dumbbell sheet, the thickness is 2.0 +/-0.2 mm, a natural ventilation electric heating ageing oven is adopted, the replacement frequency of air in the ageing oven per hour is 8-20 times, the test temperatures are 180 +/-2 ℃ and 165 +/-2 ℃, the sample is placed on a stainless steel flat plate with talcum powder spread in the ageing oven, the test temperatures are 150 +/-2 ℃ and 135 +/-2 ℃, the sample is vertically hung in an effective working area in the middle of the ageing oven, and after ageing at 4 temperature points, the service life of the nuclear power thermoplastic halogen-free flame-retardant sheath material is deduced according to the Allen niusux formula.
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