CN101565526B - Thermal anti-oxidation radiation resistance polyolefine thermal contraction material and preparation method thereof - Google Patents
Thermal anti-oxidation radiation resistance polyolefine thermal contraction material and preparation method thereof Download PDFInfo
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Abstract
A thermal anti-oxidation radiation resistance polyolefine thermal contraction material, comprising the following components by weight part: linear low density polyethylene 100-150 part, ethylene copolymer 30-80 part, polyolefine elastomer 20-40 part, cross-link sensibilizer 1-3 part, composite antioxidant 1-10 part, light stabilizer 1-5 part, halogen-containing fire retardant 20-60 part and antimony trioxide 10-30 part. The material is not only used in the nuclear island of the nuclear power station, but also widely used in the fields with higher material performance requirement such as navigation, shipping, nuclear submarine or the like.
Description
Technical field
The present invention relates to a kind of heat-shrinkage material; Relate in particular to a kind of cross-linked polyolefin heat-shrinkage material of heat-proof aging gamma ray resistant; This kind material uses in not only can be in nuclear island of nuclear power station, and can be widely applied to aviation, warship, nuclear-propelled submarine etc. to material performance requirement than higher occasion.
Background technology
Crosslinked heat-shrink tube has characteristics such as heatproof, anti-solvent, heat shrink; Be widely used in every field such as electronics, electrical equipment, space flight, aviation, locomotive, boats and ships, automobile, medical treatment, electric power, communication, pipeline, play effects such as insulating protection, waterproof sealing, reinforcement sign.Its use range arrives power cable, metallic conduit greatly, little various wire harness in the electronic product.
Can make the polyolefine material linearity molecular structure be converted into tridimensional network through certain method, take place crosslinkedly, the performance of macromolecular material at aspects such as physical strength, heatproof, chemically-resistant solvent, heat-proof agings after crosslinked all obtains very big improvement.Macromolecular material after crosslinked is heated to certain temperature when above, becomes elastomerics, expansion under external force or stretch and cooling rapidly, and this state just is retained, and when being heated to a certain temperature once more, also can return to the state before the external force effect.Utilize this characteristic of macromolecular material to can be made into various pyrocondensation devices.
In some special use occasions, have higher requirements for the radiation resistance heat-proof aging of material contracting with heat, as in the Nuclear power plants island with pyrocondensation electric cable fitting product.Pyrocondensation cable accessory in the Nuclear power plants island is because its field of employment envrionment conditions is more special; The requirement of secure context is very high; Both required not only to have good electric property, mechanical and physical performance and the flame retardant properties that general pyrocondensation annex is had, also should have long work-ing life and radiation resistance.At the Nuclear power plants run duration, the pyrocondensation cable accessory is accepted the gamma-rays radiation dose of 0.1Gy/h continuously in the nuclear island, and integrated radiation dose is about 40kGy in 40 years, and radiation dose can reach 2000kGy under the accident environment.After accepting total build-up radiation metering, cable accessory should still can keep electric property.Yet present heat-shrink tube is short work-ing life, can't reach the 90 ℃ of following work-ing lifes in 40 years of temperature, and reaches under the situation of 2000kGy heat-shrink tube loss of function property bearing gamma-rays.
Summary of the invention
The technical problem that the present invention will solve is: it is short work-ing life to overcome existing material contracting with heat; The problem of gamma ray resistant x radiation x not; Provide a kind of and can reach 40 years 90 ℃ of following work-ing lifes, the exsertile thermal anti-oxidation radiation resistance polyolefine thermal contraction material of radiation resistance, it can be applicable to occasion that material work-ing life and radiation resistance are had relatively high expectations.The present invention also further proposes the preparation method of this thermal anti-oxidation radiation resistance polyolefine thermal contraction material.
In order to solve the problems of the technologies described above, the present invention proposes following technical scheme: a kind of thermal anti-oxidation radiation resistance polyolefine thermal contraction material, and it is made up of following component according to the weight meter: 100～150 parts of linear low density polyethylenes; 30～80 parts of Injecatable EVA Copolymers; 20～40 parts of second third elastomerics or ethylene-octene copolymers; 1～3 part of multifunctional acrylate monomer; 1～10 part of composite antioxidant; 1～5 part of photostabilizer; 20～60 parts of halogen containing flame-retardants; 10～30 parts of Antimony Trioxide: 99.5Mins; The vinyl acetate content of therein ethylene-acetate ethylene copolymer is 14～30%, and melt index is 3.0～50g/10min; Described second third elastomerics comprises ethylene propylene rubber; Ice alkene type terpolymer EP rubber falls in ethylidene (ethylidene); The dicyclopentadiene type terpolymer EP rubber; Wherein ethylene content is 50～80% in second third elastomerics or the ethylene-octene copolymer; Above-mentioned multifunctional acrylate monomer is made up of in the following material one or more: the 1,3 butylene glycol dimethacrylate; 1,3 butyleneglycol diacrylate; The trihydroxy-propane trimethyl acrylic ester; The trihydroxy methyl propane triacrylate; Pentaerythritol triacrylate; The tripropylene glycol propenoate; Above-mentioned composite antioxidant is Hinered phenols antioxidant, 4: 1 composite forming of ester kind antioxidant mass ratio, and said Hinered phenols antioxidant is made up of in the following material one or more: 4,4 '-thiobis (the 6-tertiary butyl-3 methylphenol or 6-tertiary butyl cresols); 4,4 '-sulphur di-(the 6-tertiary butyl-2-methylphenol); 2,4, the 6-tri-butyl-phenol; 2,2 ,-sulfo--two (4-methyl-6-tert butyl phenol); Said ester kind antioxidant is made up of in the following material one or more: pentaerythritol tetrathioglycollate; Tyox B; The thio-2 acid stearyl; The two tetradecyl alcohol esters of thio-2 acid; Above-mentioned photostabilizer is poly-succinic (4-hydroxyl-2,2,6, a 6-tetramethyl--1-piperidines ethanol) ester, perhaps gather-{ [6-[(1; 1,3, the 3-tetramethyl butyl)-imino-]-1,3; 5-triazine-2,4-two bases] [2-(2,2,6; The 6-tetramethyl-piperidyl)-amino]-hexylidene-[4-(2,2,6, the 6-tetramethyl-piperidyl)-imino-] }.
Preferably, said halogen containing flame-retardant is chlorine-containing flame retardant or brominated flame-retardant, is made up of in the following material one or more: clorafin; Tetrachlorobisphenol A; Two bromopropyl butene dioic acid esters; Decabromodiphenyl oxide; TDE; Tetrabromoethane; Tetrabromophthalic anhydride; Three (2, the 3-dibromopropyl) SULPHOSUCCINIC ACID ESTER.
In order to solve the problems of the technologies described above, the present invention proposes following technical scheme: a kind of preparation method of thermal anti-oxidation radiation resistance polyolefine thermal contraction material, and it may further comprise the steps:
Step 1: with linear low density polyethylene, Injecatable EVA Copolymer, second third elastomerics or ethylene-octene copolymer, multifunctional acrylate monomer, composite antioxidant, photostabilizer, halogen containing flame-retardant, Antimony Trioxide: 99.5Min proportioning according to a certain percentage; Use the mixer mixing plasticizing at a certain temperature; Use mill to approach and lead to twice, use the twin screw extruder granulation to obtain the material of particulate state form;
Step 2: as required, use forming machine to make the device of different shape;
Step 3: to the device application electron beam irradiation, irradiation dose is 100～150kGy, and the macromolecular structure of material takes place crosslinked behind the irradiation;
Step 4: under 100～150 ℃, utilize the method expansion device of air pressure or machinery, make its size conforms design requirements, use water-cooled or other type of cooling flash cooler spares and make its typing, can obtain to have the macromolecular material device of thermal contraction performance.
The present invention has following beneficial effect: utilize heat-shrinkage material of the present invention can make all kinds of pyrocondensation devices, under the low dosage electron beam irradiation, material takes place crosslinked, and performance improves.When receiving the gamma-ray irradiation of high dosage, the composite antioxidant system plays a role, and reduces the Degradation of gamma-rays to material greatly.Material can keep certain mechanics and electric property.Material is after receiving the gamma-ray irradiation of 2000kGy, and breaking tenacity is greater than 5MPa, and elongation at break is greater than 50%, and volume specific resistance is greater than 10
13Ω cm.175 ℃ of thermal ageings are after 200 hours, and breaking tenacity is greater than 7MPa, and elongation at break is greater than 100%.
This material contracting with heat can use 40 years down at 90 ℃, and after receiving the gamma-ray irradiation that radiation dose is 2000kGy, the pyrocondensation device that materials used is made can keep holding its electric property.
It is 40 years that thermal anti-oxidation radiation resistance polyolefine thermal contraction material through the present invention preparation can be used for requiring 90 ℃ of following work-ing lifes, bear the occasion that the gamma-rays radiation dose reaches 2000kGy.
Embodiment
The present invention will be helped to understand through following embodiment, but content of the present invention can not be limited.
Embodiment 1
100 parts of line taking property new LDPE (film grade)s, 30 parts of Injecatable EVA Copolymers, 20 parts of terpolymer EP rubbers, 1 part in trihydroxy methyl propane three vinylformic acid, 3 parts of composite antioxidants (ratio of antioxidant 300, antioxidant 1010 is 4: 1), 1 part of photostabilizer (photostabilizer 622), 20 parts of halogen containing flame-retardants (decabromodiphenyl oxide), 10 parts of Antimony Trioxide: 99.5Mins, above-mentioned materials is mixing repeatedly even until plasticizing under 150 ℃.Material is placed in the mill thin logical twice, crushing material uses twin screw extruder extruding pelletization in 100～150 ℃ of scopes of temperature range.Pellet is fed the screw extrusion press extruding pipe material, and tubing is crosslinked under the electron beam irradiation of irradiation dose 120kGy, uses the air pressure dilator that the internal diameter of tubing is drawn together to 3 times of original size, and cooling and shaping can obtain thermal contraction casing tube fast.
The performance of thermal contraction casing tube is following:
Mechanical property: breaking tenacity 12MPa, elongation at break 650%.
Electric property: volume specific resistance 1.5 * 10
13Ω cm, disruptive strength 30kv/mm.
Flame retardant resistance: oxygen index 28.
Behind the 500kGy dosage gamma-ray irradiation, breaking tenacity 9.5MPa, elongation at break 250%.Volume specific resistance 1.8 * 10
13Ω cm.
Behind the 2000kGy dosage gamma-ray irradiation, breaking tenacity 7.2MPa, elongation at break 125%.Volume specific resistance 1.9 * 10
13Ω cm.
Behind 175 ℃ of thermal aging time 200h, breaking tenacity 9.7MPa, elongation at break 550%.
Embodiment 2
150 parts of line taking property low density polyethylene (LDPE)s, 50 parts of Injecatable EVA Copolymers, 40 parts of ethylene propylene rubbers, 1 part in tripropylene glycol vinylformic acid, 10 parts of composite antioxidants (ratio of antioxidant 330, oxidation inhibitor DLDP is 4: 1), 2 parts of photostabilizers (photostabilizer 944), 40 parts of halogen containing flame-retardants (TDE), 15 parts of Antimony Trioxide: 99.5Mins, above-mentioned materials is mixing repeatedly even until plasticizing under 150 ℃.Material is placed in the mill thin logical twice, crushing material uses twin screw extruder extruding pelletization in 100～150 ℃ of scopes of temperature range.Pellet is fed the screw extrusion press extruding pipe material, and tubing is crosslinked under the electron beam irradiation of irradiation dose 130kGy, uses the air pressure dilator that the internal diameter of tubing is drawn together to 3 times of original size, and cooling and shaping can obtain thermal contraction casing tube fast.
The performance of thermal contraction casing tube is following:
Mechanical property: breaking tenacity 15MPa, elongation at break 705%.
Electric property: volume specific resistance 2.0 * 10
13Ω cm, disruptive strength 29kv/mm.
Flame retardant resistance: oxygen index 28.
Behind the 500kGy dosage gamma-ray irradiation, breaking tenacity 10MPa, elongation at break 240%.Volume specific resistance 2.3 * 10
13Ω cm.
Behind the 2000kGy dosage gamma-ray irradiation, breaking tenacity 8MPa, elongation at break 180%.Volume specific resistance 2.5 * 10
13Ω cm.
Behind 175 ℃ of thermal aging time 200h, breaking tenacity 11MPa, elongation at break 606%.
Embodiment 3
130 parts of line taking property low density polyethylene (LDPE)s, 80 parts of Injecatable EVA Copolymers, ethene-30 parts of 1-octene copolymers, 2 parts of trihydroxy-propane trimethyl acrylic esters, 6 parts of composite antioxidants (oxidation inhibitor 736 is 4: 1 with the ratio of oxidation inhibitor DLDP), 4 parts of photostabilizers (photostabilizer 622), 60 parts of halogen containing flame-retardants (tetrabromoethane), 20 parts of Antimony Trioxide: 99.5Mins, above-mentioned materials is mixing repeatedly even until plasticizing under 150 ℃.Material is placed in the mill thin logical twice, crushing material uses twin screw extruder extruding pelletization in 100～150 ℃ of scopes of temperature range.Pellet is fed the screw extrusion press extruding pipe material, and tubing is crosslinked under the electron beam irradiation of irradiation dose 140kGy, uses the air pressure dilator that the internal diameter of tubing is drawn together to 3 times of original size, and cooling and shaping can obtain thermal contraction casing tube fast.
The performance of thermal contraction casing tube is following:
Mechanical property: breaking tenacity 13MPa, elongation at break 720%.
Electric property: volume specific resistance 2.5 * 10
13Ω cm, disruptive strength 32kv/mm.
Flame retardant resistance: oxygen index 28.
Behind the 500kGy dosage gamma-ray irradiation, breaking tenacity 10MPa, elongation at break 221%.Volume specific resistance 2.6 * 10
13Ω cm.
Behind the 2000kGy dosage gamma-ray irradiation, breaking tenacity 8MPa, elongation at break 190%.Volume specific resistance 2.8 * 10
13Ω cm.
Behind 175 ℃ of thermal aging time 200h, breaking tenacity 10MPa, elongation at break 558%.
Embodiment 4
140 parts of line taking property low density polyethylene (LDPE)s, 60 parts of Injecatable EVA Copolymers, 30 parts of terpolymer EP rubbers, 3 parts of trihydroxy methyl propane triacrylate, 4 parts of composite antioxidants (ratio of antioxidant 330 and oxidation inhibitor DSTP is 4: 1), 5 parts of photostabilizers (photostabilizer 944), 50 parts of halogen containing flame-retardants (tetrabromophthalic anhydride), 30 parts of Antimony Trioxide: 99.5Mins, above-mentioned materials is mixing repeatedly even until plasticizing under 150 ℃.Material is placed in the mill thin logical twice, crushing material uses twin screw extruder extruding pelletization in 100～150 ℃ of scopes of temperature range.Pellet is fed the screw extrusion press extruding pipe material, and tubing is crosslinked under the electron beam irradiation of irradiation dose 150kGy, uses the air pressure dilator that the internal diameter of tubing is drawn together to 3 times of original size, and cooling and shaping can obtain thermal contraction casing tube fast.
The performance of thermal contraction casing tube is following:
Mechanical property: breaking tenacity 14MPa, elongation at break 756%.
Electric property: volume specific resistance 5.4 * 10
13Ω cm, disruptive strength 30kv/mm.
Flame retardant resistance: oxygen index 28.
Behind the 500kGy dosage gamma-ray irradiation, breaking tenacity 12MPa, elongation at break 320%.Volume specific resistance 5.9 * 10
13Ω cm.
Behind the 2000kGy dosage gamma-ray irradiation, breaking tenacity 7MPa, elongation at break 200%.Volume specific resistance 5.6 * 10
13Ω cm.
Behind 175 ℃ of thermal aging time 200h, breaking tenacity 10MPa, elongation at break 600%.
Embodiment 5
120 parts of line taking property low density polyethylene (LDPE)s, 50 parts of Injecatable EVA Copolymers, 25 parts of ethylene propylene rubbers, 2 parts of pentaerythritol triacrylates, 1 part of composite antioxidant (antioxidant 330 and oxidation inhibitor DSTP ratio are 4: 1), 3 parts of photostabilizers (photostabilizer 944), 40 parts of halogen containing flame-retardants (TDE), 20 parts of Antimony Trioxide: 99.5Mins, above-mentioned materials is mixing repeatedly even until plasticizing under 150 ℃.Material is placed in the mill thin logical twice, crushing material uses twin screw extruder extruding pelletization in 100～150 ℃ of scopes of temperature range.Pellet is fed the screw extrusion press extruding pipe material, and tubing is crosslinked under the electron beam irradiation of irradiation dose 100kGy, uses the air pressure dilator that the internal diameter of tubing is drawn together to 3 times of original size, and cooling and shaping can obtain thermal contraction casing tube fast.
The performance of thermal contraction casing tube is following:
Mechanical property: breaking tenacity 15MPa, elongation at break 690%.
Electric property: volume specific resistance 4 * 10
13Ω cm, disruptive strength 35kv/mm.
Flame retardant resistance: oxygen index 28.
Behind the 500kGy dosage gamma-ray irradiation, breaking tenacity 12MPa, elongation at break 258%.Volume specific resistance 4.1 * 10
13Ω cm.
Behind the 2000kGy dosage gamma-ray irradiation, breaking tenacity 7.5MPa, elongation at break 130%.Volume specific resistance 4.3 * 10
13Ω cm.
Behind 175 ℃ of thermal aging time 200h, breaking tenacity 12MPa, elongation at break 540%.
Utilize heat-shrinkage material of the present invention can make all kinds of pyrocondensation devices, under the low dosage electron beam irradiation, material takes place crosslinked, and performance improves.When receiving the gamma-ray irradiation of high dosage, material can keep certain mechanics and electric property.Material is after receiving the 2000kGy gamma-ray irradiation, and breaking tenacity is greater than 5MPa, and elongation at break is greater than 50%, and volume specific resistance is greater than 10
13Ω cm.175 ℃ of thermal ageings are after 200 hours, and breaking tenacity is greater than 7MPa, and elongation at break is greater than 100%.
This material contracting with heat can use 40 years down at 90 ℃, and after receiving the gamma-ray irradiation that radiation dose is 2000kGy, the pyrocondensation device that materials used is made can keep holding its electric property.
Claims (3)
1. thermal anti-oxidation radiation resistance polyolefine thermal contraction material, it is made up of following component according to the weight meter:
100～150 parts of linear low density polyethylenes;
30～80 parts of Injecatable EVA Copolymers;
20～40 parts of second third elastomerics or ethylene-octene copolymers;
1～3 part of multifunctional acrylate monomer;
1～10 part of composite antioxidant;
1～5 part of photostabilizer;
20～60 parts of halogen containing flame-retardants;
10～30 parts of Antimony Trioxide: 99.5Mins;
The vinyl acetate content of therein ethylene-acetate ethylene copolymer is 14～30%, and melt index is 3.0～50g/10min;
Described second third elastomerics comprises ethylene propylene rubber; Ice alkene type terpolymer EP rubber falls in ethylidene (ethylidene); The dicyclopentadiene type terpolymer EP rubber;
Wherein ethylene content is 50～80% in second third elastomerics or the ethylene-octene copolymer;
Above-mentioned multifunctional acrylate monomer is made up of in the following material one or more: the 1,3 butylene glycol dimethacrylate; 1,3 butyleneglycol diacrylate; The trihydroxy-propane trimethyl acrylic ester; The trihydroxy methyl propane triacrylate; Pentaerythritol triacrylate; The tripropylene glycol propenoate;
Above-mentioned composite antioxidant is Hinered phenols antioxidant, 4: 1 composite forming of ester kind antioxidant mass ratio, and said Hinered phenols antioxidant is made up of in the following material one or more: 4,4 '-thiobis (the 6-tertiary butyl-3 methylphenol or 6-tertiary butyl cresols); 4,4 '-sulphur di-(the 6-tertiary butyl-2-methylphenol); 2,4, the 6-tri-butyl-phenol; 2,2 ,-sulfo--two (4-methyl-6-tert butyl phenol); Said ester kind antioxidant is made up of in the following material one or more: pentaerythritol tetrathioglycollate; Tyox B; The thio-2 acid stearyl; The two tetradecyl alcohol esters of thio-2 acid;
Above-mentioned photostabilizer is poly-succinic (4-hydroxyl-2,2,6, a 6-tetramethyl--1-piperidines ethanol) ester, perhaps gather-{ [6-[(1; 1,3, the 3-tetramethyl butyl)-imino-]-1,3; 5-triazine-2,4-two bases] [2-(2,2,6; The 6-tetramethyl-piperidyl)-amino]-hexylidene-[4-(2,2,6, the 6-tetramethyl-piperidyl)-imino-] }.
2. thermal anti-oxidation radiation resistance polyolefine thermal contraction material according to claim 1 is characterized in that: said halogen containing flame-retardant is chlorine-containing flame retardant or brominated flame-retardant, is made up of in the following material one or more: clorafin; Tetrachlorobisphenol A; Two bromopropyl butene dioic acid esters; Decabromodiphenyl oxide; TDE; Tetrabromoethane; Tetrabromophthalic anhydride; Three (2, the 3-dibromopropyl) SULPHOSUCCINIC ACID ESTER.
3. preparation method who prepares thermal anti-oxidation radiation resistance polyolefine thermal contraction material as claimed in claim 1, it may further comprise the steps:
Step 1: with linear low density polyethylene, Injecatable EVA Copolymer, second third elastomerics or ethylene-octene copolymer, multifunctional acrylate monomer, composite antioxidant, photostabilizer, halogen containing flame-retardant, Antimony Trioxide: 99.5Min proportioning according to a certain percentage; Use the mixer mixing plasticizing at a certain temperature; Use mill to approach and lead to twice, use the twin screw extruder granulation to obtain the material of particulate state form;
Step 2: as required, use forming machine to make the device of different shape;
Step 3: to the device application electron beam irradiation, irradiation dose is 100～150kGy, and the macromolecular structure of material takes place crosslinked behind the irradiation;
Step 4: under 100～150 ℃, utilize the method expansion device of air pressure or machinery, make its size conforms design requirements, use water-cooled or other type of cooling flash cooler spares and make its typing, can obtain to have the macromolecular material device of thermal contraction performance.
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