CN103435901A - Ultraviolet crosslinking low-smoke halogen-free flame-retardant polyolefin insulating material and preparation method thereof - Google Patents
Ultraviolet crosslinking low-smoke halogen-free flame-retardant polyolefin insulating material and preparation method thereof Download PDFInfo
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- CN103435901A CN103435901A CN2013104162513A CN201310416251A CN103435901A CN 103435901 A CN103435901 A CN 103435901A CN 2013104162513 A CN2013104162513 A CN 2013104162513A CN 201310416251 A CN201310416251 A CN 201310416251A CN 103435901 A CN103435901 A CN 103435901A
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Abstract
The invention relates to an ultraviolet crosslinking low-smoke halogen-free flame-retardant polyolefin insulating material and a preparation method thereof, and specifically relates to the ultraviolet crosslinking low-smoke halogen-free flame-retardant polyolefin insulating material for manufacturing insulating layers of flame-retardant wires and cables, and a preparation method of the insulating material. The ultraviolet crosslinking low-smoke halogen-free flame-retardant polyolefin insulating material is prepared by mixing raw materials including linear low-density polyethylene resin, ethylene-vinyl acetate copolymer resin, a halogen-free flame retardant, a flame-retardant synergist, a cation photoinitiator, a free radical photoinitiator, a crosslinking agent, an antioxidant, a lubricant and the like in a closed mixing mill of which the temperature is 130-140 DEG C, and then extruding the mixture in a twin-screw extruder with six temperature sections. By adopting the ultraviolet crosslinking low-smoke halogen-free flame-retardant polyolefin insulating material provided by the invention, the defects of three crosslinking methods are avoided, and the advantages of high production efficiency, simple process, small equipment investment, economical efficiency, energy conservation, environmental protection, wide adaptability, good product performance stability and the like are achieved.
Description
Technical field
The present invention relates to a kind of plastic pellet and preparation method thereof.Specifically, be the ultraviolet light cross-linking low smoke halogen-free flame-retardant polyolefin Insulating Material and Preparation Method of making the flame-retardant electric wire and cable insulation layer.
Background technology
In recent years, along with the develop rapidly of the relevant industries such as electric power, motor, electronic apparatus, automobile, require cross-linked wire and cable to there are the characteristics such as excellent heat resistance, good, withstand voltage broken, the anti-solvent of stress cracking resistance, the welding of anti-flatiron, long service life.At present, cross-linked wire and cable has been successfully used to motor lead, electric mounting line, automotive line, locomotive wire, line for building, warship wire for ship, petroleum industry cable, the aspects such as overhead line.With regard to the insulating material kind of its use, with cross-linking polyolefin insulation electric wire cable consumption maximum.At present, cross-linking polyolefin insulation electric wire cable preparation method has three kinds of general cross-linking methods: superoxide chemical crosslink technique, high-energy radiation crosslinking, silane cross-linking method.Wherein, the deficiency that the superoxide chemical crosslink technique exists is that its production efficiency is low, technical process is complicated, power consumption is large, the efficiency utilization ratio is low, the product scrap rate is high; The facility investment of high-energy radiation crosslinking is large, Operation and Maintenance is complicated, protection condition harshness, and because its process characteristic is only suitable for making the electric wire that wall thickness is thinner, and the uniformity of radiation of heavy wall electric wire is bad; Silane cross-linking method relates to hydrolysis reaction, and the electric wire poor stability, withstand voltage and temperature resistant grade is lower, be not suitable for doing the halogen-free flame-retardant wire cable.
Summary of the invention
The problem that the present invention will solve is to provide a kind of ultraviolet light cross-linking low smoke halogen-free flame-retardant polyolefin Insulation Material.Adopt ultraviolet light cross-linking low smoke halogen-free flame-retardant polyolefin Insulation Material of the present invention, avoid the deficiency of above-mentioned three kinds of cross-linking methods, there is the advantages such as production efficiency is high, technique is simple, facility investment is little, economy, energy-conserving and environment-protective, wide adaptability, product performance good stability.
Another problem that the present invention will solve is to provide a kind of method for preparing ultraviolet light cross-linking low smoke halogen-free flame-retardant polyolefin Insulation Material.
For addressing the above problem, taked following technical scheme:
Ultraviolet light cross-linking low smoke halogen-free flame-retardant polyolefin Insulation Material characteristics of the present invention are the raw materials that comprise following parts by weight:
Linear low density polyethylene resin 30 ~ 40 weight parts;
Ethylene-vinyl acetate copolymer resins 60 ~ 70 weight parts;
Halogen-free flame retardants 50 ~ 60 weight parts;
Fire retarding synergist 10 ~ 15 weight parts;
Cation light initiator 0.5 ~ 0.8 weight part;
Free radical photo-initiation 2 ~ 5 weight parts;
Linking agent 1.0 ~ 1.5 weight parts;
Oxidation inhibitor 0.5 ~ 1.0 weight part;
Lubricant 1 ~ 1.5 weight part.
Wherein:
In described ethylene-vinyl acetate copolymer resins, the content of vinyl acetate between to for plastic is 26 ~ 28%, melting index≤6g/10min;
Described halogen-free flame retardants is with ammonium polyphosphate, 3.5 hydrate zinc borates, tetramethylolmethane, trimeric cyanamide, and according to ammonium polyphosphate: the part by weight of 3.5 hydrate zinc borates: tetramethylolmethane: trimeric cyanamide=3.8:1.2:1.0:1.2 mixes;
Described fire retarding synergist is silica flour modified resin, and it is the RM 4-7081 type silica flour modified resin that U.S. Dow Corning company produces;
Described cation light initiator is with cyclopentadiene isopropyl benzene iron hexafluorophosphate and diphenyl iodine hexafluorophosphate, and according to cyclopentadiene isopropyl benzene iron hexafluorophosphate: the part by weight of diphenyl iodine hexafluorophosphate=3:1 mixes;
Described free radical photo-initiation is by 2-methyl isophthalic acid-(4-methylthio group phenyl)-2-morpholinyl-1-acetone and benzophenone, and mixes according to the part by weight of 2-methyl isophthalic acid-(4-methylthio group phenyl)-2-morpholinyl-1-acetone: benzophenone=5:3.
Described linking agent is cyanacrylate;
Described oxidation inhibitor be four [3-(3 ', 5 '-di-t-butyl-4 '-hydroxy phenyl) propionic acid] pentaerythritol ester or 2,6-bis-(1-phenyl) ethyl-4-nonylphenol.
Described lubricated employing polyethylene wax and stearic acid, and mix according to the part by weight of polyethylene wax: stearic acid=3:1.
The method for preparing described ultraviolet light cross-linking low smoke halogen-free flame-retardant polyolefin Insulation Material comprises the following steps successively:
First linear low density polyethylene resin, ethylene-vinyl acetate copolymer resins, halogen-free flame retardants, fire retarding synergist, cation light initiator, free radical photo-initiation, linking agent, oxidation inhibitor lubricant are dropped in the closed mixing machine that temperature is 130 ~ 140 ℃ together, mixing 12 ~ 15 minutes, obtain the bulk compound;
Then, described bulk compound is dropped in six temperature section twin screw extruders, extrude into the particle that particle diameter is 3 ~ 4mm, obtain ultraviolet light cross-linking low smoke halogen-free flame-retardant polyolefin Insulation Material; Wherein, the temperature of six of described six temperature section twin screw extruders temperature sections is respectively 130 ℃, 140 ℃, 145 ℃, 150 ℃, 155 ℃, 150 ℃.
Adopt such scheme, have the following advantages:
Because the halogen-free flame retardants adopted in raw material of the present invention and fire retarding synergist have excellent cooperative flame retardant effect, in the situation that the total consumption of fire retardant is few, can make the present invention reach good halogen-free flameproof effect.Because the total consumption of fire retardant is few, make the present invention easily see through at crosslinked course of processing medium ultraviolet light, can crosslinking reaction occur preferably, form even, intensive cross-linking set, be conducive to improve properties of the present invention.
In raw material of the present invention, cation light initiator adopts cyclopentadiene isopropyl benzene iron hexafluorophosphate and diphenyl iodine hexafluorophosphate to be used in conjunction with, and has taken into account the ultraviolet wavelength scope that high voltage mercury lamp sends, and has further improved ultraviolet absorption efficiency.Free radical photo-initiation adopts 2-methyl isophthalic acid-(4-methylthio group phenyl)-2-morpholinyl-1-acetone/benzophenone to be used in conjunction with, and utilizes the synergy of crack type photoinitiator and hydrogen-capture-type light initiator, to improve, causes cross-linking efficiency.
Again due in raw material of the present invention, use cation light initiator and free radical photo-initiation simultaneously, utilized different light-initiated mechanism to combine, further improved cross-linking efficiency, rate of crosslinking, the crosslinked homogeneity of product of the present invention, made product of the present invention there is stable, good withstand voltage, thermotolerance and mechanical and physical performance.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail:
Embodiment mono-
First choose crosslinked, the oxidation inhibitor of 0.5 weight part of free radical photo-initiation, 1 weight part of cation light initiator, 2 weight parts of fire retarding synergist, 0.5 weight part of halogen-free flame retardants, 10 weight parts of ethylene-vinyl acetate copolymer resins, 50 weight parts of linear low density polyethylene resin, 70 weight parts of 30 weight parts, the lubricant of 1.0 weight parts.
Then, linear low density polyethylene resin, ethylene-vinyl acetate copolymer resins, halogen-free flame retardants, fire retarding synergist, cation light initiator, free radical photo-initiation, linking agent, oxidation inhibitor lubricant are dropped in the closed mixing machine that temperature is 130 ℃ together, mixing 12 minutes, obtain the bulk compound.
Finally, described bulk compound is dropped in six temperature section twin screw extruders, extrude into the particle that particle diameter is 3mm, obtain ultraviolet light cross-linking low smoke halogen-free flame-retardant polyolefin Insulation Material.Wherein, the temperature of six of described six temperature section twin screw extruders temperature sections is respectively 130 ℃, 140 ℃, 145 ℃, 150 ℃, 155 ℃, 150 ℃.
In the present embodiment:
The melting index of described linear low density polyethylene resin is 1.0 ~ 2.0g/10min;
In described ethylene-vinyl acetate copolymer resins, the content of vinyl acetate between to for plastic is 26 ~ 28%, melting index≤6g/10min;
Described halogen-free flame retardants is with ammonium polyphosphate, 3.5 hydrate zinc borates, tetramethylolmethane, trimeric cyanamide, and according to ammonium polyphosphate: the part by weight of 3.5 hydrate zinc borates: tetramethylolmethane: trimeric cyanamide=3.8:1.2:1.0:1.2 mixes;
Described fire retarding synergist is silica flour modified resin, and it is the RM 4-7081 type silica flour modified resin that U.S. Dow Corning company produces.
Described cation light initiator is with cyclopentadiene isopropyl benzene iron hexafluorophosphate and diphenyl iodine hexafluorophosphate, and according to cyclopentadiene isopropyl benzene iron hexafluorophosphate: the part by weight of diphenyl iodine hexafluorophosphate=3:1 mixes.
Described free radical photo-initiation is by 2-methyl isophthalic acid-(4-methylthio group phenyl)-2-morpholinyl-1-acetone and benzophenone, and mixes according to the part by weight of 2-methyl isophthalic acid-(4-methylthio group phenyl)-2-morpholinyl-1-acetone: benzophenone=5:3.
Described linking agent is cyanacrylate.
Described oxidation inhibitor be four [3-(3 ', 5 '-di-t-butyl-4 '-hydroxy phenyl) propionic acid] pentaerythritol ester or 2,6-bis-(1-phenyl) ethyl-4-nonylphenol.
Described lubricant adopts polyethylene wax and stearic acid, and mixes according to the part by weight of polyethylene wax: stearic acid=3:1.
Embodiment bis-
First choose crosslinked, the oxidation inhibitor of 0.8 weight part of free radical photo-initiation, 1.2 weight parts of cation light initiator, 3.5 weight parts of fire retarding synergist, 0.6 weight part of halogen-free flame retardants, 12 weight parts of ethylene-vinyl acetate copolymer resins, 55 weight parts of linear low density polyethylene resin, 65 weight parts of 35 weight parts, the lubricant of 1.2 weight parts.
Then, linear low density polyethylene resin, ethylene-vinyl acetate copolymer resins, halogen-free flame retardants, fire retarding synergist, cation light initiator, free radical photo-initiation, linking agent, oxidation inhibitor lubricant are dropped in the closed mixing machine that temperature is 135 ℃ together, mixing 14 minutes, obtain the bulk compound.
Finally, described bulk compound is dropped in six temperature section twin screw extruders, extrude into the particle that particle diameter is 3.5mm, obtain ultraviolet light cross-linking low smoke halogen-free flame-retardant polyolefin Insulation Material.Wherein, the temperature of six of described six temperature section twin screw extruders temperature sections is respectively 130 ℃, 140 ℃, 145 ℃, 150 ℃, 155 ℃, 150 ℃.
In the present embodiment:
The melting index of described linear low density polyethylene resin is 1.0 ~ 2.0g/10min;
In described ethylene-vinyl acetate copolymer resins, the content of vinyl acetate between to for plastic is 26 ~ 28%, melting index≤6g/10min;
Described halogen-free flame retardants is with ammonium polyphosphate, 3.5 hydrate zinc borates, tetramethylolmethane, trimeric cyanamide, and according to ammonium polyphosphate: the part by weight of 3.5 hydrate zinc borates: tetramethylolmethane: trimeric cyanamide=3.8:1.2:1.0:1.2 mixes;
Described fire retarding synergist is silica flour modified resin, and it is the RM 4-7081 type silica flour modified resin that U.S. Dow Corning company produces.
Described cation light initiator is with cyclopentadiene isopropyl benzene iron hexafluorophosphate and diphenyl iodine hexafluorophosphate, and according to cyclopentadiene isopropyl benzene iron hexafluorophosphate: the part by weight of diphenyl iodine hexafluorophosphate=3:1 mixes.
Described free radical photo-initiation is by 2-methyl isophthalic acid-(4-methylthio group phenyl)-2-morpholinyl-1-acetone and benzophenone, and mixes according to the part by weight of 2-methyl isophthalic acid-(4-methylthio group phenyl)-2-morpholinyl-1-acetone: benzophenone=5:3.
Described linking agent is cyanacrylate.
Described oxidation inhibitor be four [3-(3 ', 5 '-di-t-butyl-4 '-hydroxy phenyl) propionic acid] pentaerythritol ester or 2,6-bis-(1-phenyl) ethyl-4-nonylphenol.
Described lubricant adopts polyethylene wax and stearic acid, and mixes according to the part by weight of polyethylene wax: stearic acid=3:1.
Embodiment tri-
First choose crosslinked, the oxidation inhibitor of 1.0 weight parts of free radical photo-initiation, 1.5 weight parts of cation light initiator, 5 weight parts of fire retarding synergist, 0.8 weight part of halogen-free flame retardants, 15 weight parts of ethylene-vinyl acetate copolymer resins, 60 weight parts of linear low density polyethylene resin, 60 weight parts of 40 weight parts, the lubricant of 1.5 weight parts.
Then, linear low density polyethylene resin, ethylene-vinyl acetate copolymer resins, halogen-free flame retardants, fire retarding synergist, cation light initiator, free radical photo-initiation, linking agent, oxidation inhibitor lubricant are dropped in the closed mixing machine that temperature is 140 ℃ together, mixing 15 minutes, obtain the bulk compound.
Finally, described bulk compound is dropped in six temperature section twin screw extruders, extrude into the particle that particle diameter is 3.5mm, obtain ultraviolet light cross-linking low smoke halogen-free flame-retardant polyolefin Insulation Material.Wherein, the temperature of six of described six temperature section twin screw extruders temperature sections is respectively 130 ℃, 140 ℃, 145 ℃, 150 ℃, 155 ℃, 150 ℃.
In the present embodiment:
The melting index of described linear low density polyethylene resin is 1.0 ~ 2.0g/10min;
In described ethylene-vinyl acetate copolymer resins, the content of vinyl acetate between to for plastic is 26 ~ 28%, melting index≤6g/10min;
Described halogen-free flame retardants is with ammonium polyphosphate, 3.5 hydrate zinc borates, tetramethylolmethane, trimeric cyanamide, and according to ammonium polyphosphate: the part by weight of 3.5 hydrate zinc borates: tetramethylolmethane: trimeric cyanamide=3.8:1.2:1.0:1.2 mixes;
Described fire retarding synergist is silica flour modified resin, and it is the RM 4-7081 type silica flour modified resin that U.S. Dow Corning company produces.
Described cation light initiator is with cyclopentadiene isopropyl benzene iron hexafluorophosphate and diphenyl iodine hexafluorophosphate, and according to cyclopentadiene isopropyl benzene iron hexafluorophosphate: the part by weight of diphenyl iodine hexafluorophosphate=3:1 mixes.
Described free radical photo-initiation is by 2-methyl isophthalic acid-(4-methylthio group phenyl)-2-morpholinyl-1-acetone and benzophenone, and mixes according to the part by weight of 2-methyl isophthalic acid-(4-methylthio group phenyl)-2-morpholinyl-1-acetone: benzophenone=5:3.
Described linking agent is cyanacrylate.
Described oxidation inhibitor be four [3-(3 ', 5 '-di-t-butyl-4 '-hydroxy phenyl) propionic acid] pentaerythritol ester or 2,6-bis-(1-phenyl) ethyl-4-nonylphenol.
Described lubricant adopts polyethylene wax and stearic acid, and mixes according to the part by weight of polyethylene wax: stearic acid=3:1.
Claims (10)
1. ultraviolet light cross-linking low smoke halogen-free flame-retardant polyolefin Insulation Material is characterized in that comprising the raw material of following parts by weight:
Linear low density polyethylene resin 30 ~ 40 weight parts;
Ethylene-vinyl acetate copolymer resins 60 ~ 70 weight parts;
Halogen-free flame retardants 50 ~ 60 weight parts;
Fire retarding synergist 10 ~ 15 weight parts;
Cation light initiator 0.5 ~ 0.8 weight part;
Free radical photo-initiation 2 ~ 5 weight parts;
Linking agent 1.0 ~ 1.5 weight parts;
Oxidation inhibitor 0.5 ~ 1.0 weight part;
Lubricant 1 ~ 1.5 weight part.
2. ultraviolet light cross-linking low smoke halogen-free flame-retardant polyolefin Insulation Material as claimed in claim 1, is characterized in that, in described ethylene-vinyl acetate copolymer resins, the content of vinyl acetate between to for plastic is 26 ~ 28%, melting index≤6g/10min.
3. ultraviolet light cross-linking low smoke halogen-free flame-retardant polyolefin Insulation Material as claimed in claim 1, it is characterized in that described halogen-free flame retardants is with ammonium polyphosphate, 3.5 hydrate zinc borates, tetramethylolmethane, trimeric cyanamide, and according to ammonium polyphosphate: the part by weight of 3.5 hydrate zinc borates: tetramethylolmethane: trimeric cyanamide=3.8:1.2:1.0:1.2 mixes.
4. ultraviolet light cross-linking low smoke halogen-free flame-retardant polyolefin Insulation Material as claimed in claim 1, is characterized in that described fire retarding synergist is silica flour modified resin, and it is the RM 4-7081 type silica flour modified resin that U.S. Dow Corning company produces.
5. ultraviolet light cross-linking low smoke halogen-free flame-retardant polyolefin Insulation Material as claimed in claim 1, it is characterized in that described cation light initiator is with cyclopentadiene isopropyl benzene iron hexafluorophosphate and diphenyl iodine hexafluorophosphate, and according to cyclopentadiene isopropyl benzene iron hexafluorophosphate: the part by weight of diphenyl iodine hexafluorophosphate=3:1 mixes.
6. ultraviolet light cross-linking low smoke halogen-free flame-retardant polyolefin Insulation Material as claimed in claim 1, it is characterized in that described free radical photo-initiation is by 2-methyl isophthalic acid-(4-methylthio group phenyl)-2-morpholinyl-1-acetone and benzophenone, and mix according to the part by weight of 2-methyl isophthalic acid-(4-methylthio group phenyl)-2-morpholinyl-1-acetone: benzophenone=5:3.
7. ultraviolet light cross-linking low smoke halogen-free flame-retardant polyolefin Insulation Material as claimed in claim 1, is characterized in that described linking agent is cyanacrylate.
8. ultraviolet light cross-linking low smoke halogen-free flame-retardant polyolefin Insulation Material as claimed in claim 1, it is characterized in that described oxidation inhibitor be four [3-(3 ', 5 '-di-t-butyl-4 '-hydroxy phenyl) propionic acid] pentaerythritol ester or 2,6-bis-(1-phenyl) ethyl-4-nonylphenol.
9. ultraviolet light cross-linking low smoke halogen-free flame-retardant polyolefin Insulation Material as claimed in claim 1, is characterized in that described lubricant adopts polyethylene wax and stearic acid and mixes according to the part by weight of polyethylene wax: stearic acid=3:1.
10. prepare the method for the described ultraviolet light cross-linking low smoke halogen-free flame-retardant polyolefin of claim 1 Insulation Material, it is characterized in that comprising the following steps successively:
First by linear low density polyethylene resin, ethylene-vinyl acetate copolymer resins, halogen-free flame retardants, fire retarding synergist, cation light initiator, free radical photo-initiation, linking agent, oxidation inhibitor
,lubricant drops in the closed mixing machine that temperature is 130 ~ 140 ℃ together, mixing 12 ~ 15 minutes, obtains the bulk compound;
Then, described bulk compound is dropped in six temperature section twin screw extruders, extrude into the particle that particle diameter is 3 ~ 4mm, obtain ultraviolet light cross-linking low smoke halogen-free flame-retardant polyolefin Insulation Material; Wherein, the temperature of six of described six temperature section twin screw extruders temperature sections is respectively 130 ℃, 140 ℃, 145 ℃, 150 ℃, 155 ℃, 150 ℃.
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CN103819897A (en) * | 2014-01-26 | 2014-05-28 | 成都玉龙化工有限公司 | Nitrogen flame retardant, preparation thereof and flame-retardant silicone rubber compound |
CN109705441A (en) * | 2018-11-20 | 2019-05-03 | 上海至正道化高分子材料股份有限公司 | 150 DEG C of ultraviolet light cross-linking low smoke and low halogen CABLE MATERIALSs of one kind and preparation method thereof |
CN110577697A (en) * | 2019-09-20 | 2019-12-17 | 江苏德威新材料股份有限公司 | UVLED light attenuation irradiation resistant crosslinked polyethylene insulation master batch and preparation method and application thereof |
CN110790997A (en) * | 2018-10-12 | 2020-02-14 | 山西山花新材料有限公司 | Ultraviolet crosslinkable polyethylene cable insulation material prepared by adsorption method |
CN110982157A (en) * | 2019-12-25 | 2020-04-10 | 上海新上化高分子材料有限公司 | Low-odor rapid UV-LED ultraviolet light crosslinked polyethylene insulating material and preparation method thereof |
CN113402805A (en) * | 2021-06-17 | 2021-09-17 | 成都鑫成鹏高分子科技股份有限公司 | Ultraviolet light fast crosslinking high-flame-retardant low-smoke halogen-free insulating material and preparation method thereof |
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CN103819897A (en) * | 2014-01-26 | 2014-05-28 | 成都玉龙化工有限公司 | Nitrogen flame retardant, preparation thereof and flame-retardant silicone rubber compound |
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CN110790997A (en) * | 2018-10-12 | 2020-02-14 | 山西山花新材料有限公司 | Ultraviolet crosslinkable polyethylene cable insulation material prepared by adsorption method |
CN109705441A (en) * | 2018-11-20 | 2019-05-03 | 上海至正道化高分子材料股份有限公司 | 150 DEG C of ultraviolet light cross-linking low smoke and low halogen CABLE MATERIALSs of one kind and preparation method thereof |
CN110577697A (en) * | 2019-09-20 | 2019-12-17 | 江苏德威新材料股份有限公司 | UVLED light attenuation irradiation resistant crosslinked polyethylene insulation master batch and preparation method and application thereof |
CN110982157A (en) * | 2019-12-25 | 2020-04-10 | 上海新上化高分子材料有限公司 | Low-odor rapid UV-LED ultraviolet light crosslinked polyethylene insulating material and preparation method thereof |
CN113402805A (en) * | 2021-06-17 | 2021-09-17 | 成都鑫成鹏高分子科技股份有限公司 | Ultraviolet light fast crosslinking high-flame-retardant low-smoke halogen-free insulating material and preparation method thereof |
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Application publication date: 20131211 |