CN114163716B - High carbon black photo-oxidative aging resistant silane crosslinked polyethylene insulating material and preparation method thereof - Google Patents
High carbon black photo-oxidative aging resistant silane crosslinked polyethylene insulating material and preparation method thereof Download PDFInfo
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- CN114163716B CN114163716B CN202111609244.6A CN202111609244A CN114163716B CN 114163716 B CN114163716 B CN 114163716B CN 202111609244 A CN202111609244 A CN 202111609244A CN 114163716 B CN114163716 B CN 114163716B
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- 239000006229 carbon black Substances 0.000 title claims abstract description 74
- 239000004718 silane crosslinked polyethylene Substances 0.000 title claims abstract description 21
- 239000011810 insulating material Substances 0.000 title claims abstract description 13
- 230000032683 aging Effects 0.000 title abstract description 20
- 238000002360 preparation method Methods 0.000 title abstract description 9
- 239000011347 resin Substances 0.000 claims abstract description 30
- 229920005989 resin Polymers 0.000 claims abstract description 30
- 239000000463 material Substances 0.000 claims abstract description 22
- 239000003607 modifier Substances 0.000 claims abstract description 16
- 229920000092 linear low density polyethylene Polymers 0.000 claims abstract description 15
- 239000004707 linear low-density polyethylene Substances 0.000 claims abstract description 15
- 239000002131 composite material Substances 0.000 claims abstract description 14
- 239000004094 surface-active agent Substances 0.000 claims abstract description 12
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 9
- 239000004611 light stabiliser Substances 0.000 claims abstract description 9
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 6
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 6
- 239000003054 catalyst Substances 0.000 claims abstract description 6
- 229920001684 low density polyethylene Polymers 0.000 claims abstract description 6
- 239000004702 low-density polyethylene Substances 0.000 claims abstract description 6
- 239000003999 initiator Substances 0.000 claims abstract description 3
- 239000006254 rheological additive Substances 0.000 claims abstract description 3
- 238000002156 mixing Methods 0.000 claims description 18
- 238000001035 drying Methods 0.000 claims description 17
- 239000002245 particle Substances 0.000 claims description 12
- -1 3, 5-di-tert-butyl-4-hydroxyphenyl Chemical group 0.000 claims description 11
- 239000004594 Masterbatch (MB) Substances 0.000 claims description 11
- 206010051246 Photodermatosis Diseases 0.000 claims description 11
- 230000008845 photoaging Effects 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 7
- 239000007822 coupling agent Substances 0.000 claims description 6
- 238000001125 extrusion Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000012545 processing Methods 0.000 claims description 6
- 238000009413 insulation Methods 0.000 claims description 5
- XOUQAVYLRNOXDO-UHFFFAOYSA-N 2-tert-butyl-5-methylphenol Chemical compound CC1=CC=C(C(C)(C)C)C(O)=C1 XOUQAVYLRNOXDO-UHFFFAOYSA-N 0.000 claims description 4
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 4
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 4
- 239000000155 melt Substances 0.000 claims description 4
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical group C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 claims description 3
- 239000004712 Metallocene polyethylene (PE-MC) Substances 0.000 claims description 3
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical group CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 3
- 238000007664 blowing Methods 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 239000012975 dibutyltin dilaurate Substances 0.000 claims description 3
- 239000004615 ingredient Substances 0.000 claims description 3
- 229920001912 maleic anhydride grafted polyethylene Polymers 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 claims description 3
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 2
- 239000004698 Polyethylene Substances 0.000 claims description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- 150000001412 amines Chemical class 0.000 claims description 2
- AGXUVMPSUKZYDT-UHFFFAOYSA-L barium(2+);octadecanoate Chemical compound [Ba+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O AGXUVMPSUKZYDT-UHFFFAOYSA-L 0.000 claims description 2
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 2
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims description 2
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical group CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 claims description 2
- WOXXJEVNDJOOLV-UHFFFAOYSA-N ethenyl-tris(2-methoxyethoxy)silane Chemical compound COCCO[Si](OCCOC)(OCCOC)C=C WOXXJEVNDJOOLV-UHFFFAOYSA-N 0.000 claims description 2
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 2
- 239000000347 magnesium hydroxide Substances 0.000 claims description 2
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 2
- 229920000573 polyethylene Polymers 0.000 claims description 2
- 125000001501 propionyl group Chemical group O=C([*])C([H])([H])C([H])([H])[H] 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 239000012774 insulation material Substances 0.000 claims 5
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 claims 1
- 239000004811 fluoropolymer Substances 0.000 claims 1
- 229920002313 fluoropolymer Polymers 0.000 claims 1
- NFHFRUOZVGFOOS-UHFFFAOYSA-N palladium;triphenylphosphane Chemical compound [Pd].C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 NFHFRUOZVGFOOS-UHFFFAOYSA-N 0.000 claims 1
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 claims 1
- 229920001296 polysiloxane Polymers 0.000 claims 1
- 239000011159 matrix material Substances 0.000 abstract description 10
- 239000000126 substance Substances 0.000 abstract description 8
- 238000005336 cracking Methods 0.000 abstract description 6
- 230000004048 modification Effects 0.000 abstract description 6
- 238000012986 modification Methods 0.000 abstract description 6
- 230000009471 action Effects 0.000 abstract description 5
- 230000007774 longterm Effects 0.000 abstract description 4
- 235000019241 carbon black Nutrition 0.000 description 49
- 230000000052 comparative effect Effects 0.000 description 10
- 238000012360 testing method Methods 0.000 description 7
- 230000008569 process Effects 0.000 description 4
- 230000006353 environmental stress Effects 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 2
- 238000002715 modification method Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 238000004381 surface treatment Methods 0.000 description 2
- HCILJBJJZALOAL-UHFFFAOYSA-N 3-(3,5-ditert-butyl-4-hydroxyphenyl)-n'-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyl]propanehydrazide Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)NNC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 HCILJBJJZALOAL-UHFFFAOYSA-N 0.000 description 1
- WPMYUUITDBHVQZ-UHFFFAOYSA-N 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoic acid Chemical compound CC(C)(C)C1=CC(CCC(O)=O)=CC(C(C)(C)C)=C1O WPMYUUITDBHVQZ-UHFFFAOYSA-N 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000003679 aging effect Effects 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229920001400 block copolymer Polymers 0.000 description 1
- 159000000007 calcium salts Chemical class 0.000 description 1
- 150000001721 carbon Chemical class 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 229920003020 cross-linked polyethylene Polymers 0.000 description 1
- 239000004703 cross-linked polyethylene Substances 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000009778 extrusion testing Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000007781 pre-processing Methods 0.000 description 1
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 150000003751 zinc Chemical class 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/08—Copolymers of ethene
- C08L23/0807—Copolymers of ethene with unsaturated hydrocarbons only containing more than three carbon atoms
- C08L23/0815—Copolymers of ethene with aliphatic 1-olefins
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
- H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
- H01B3/30—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes
- H01B3/44—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes vinyl resins; acrylic resins
- H01B3/441—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes vinyl resins; acrylic resins from alkenes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/2224—Magnesium hydroxide
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K2201/011—Nanostructured additives
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/202—Applications use in electrical or conductive gadgets use in electrical wires or wirecoating
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2312/00—Crosslinking
- C08L2312/08—Crosslinking by silane
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Abstract
The invention relates to a high carbon black photo-oxidative aging resistant silane crosslinked polyethylene insulating material and a preparation method thereof, wherein the high carbon black photo-oxidative aging resistant silane crosslinked polyethylene insulating material is prepared from linear low-density polyethylene resin A, linear low-density polyethylene resin B, high-pressure low-density polyethylene, a silane coupling agent, an initiator, an antioxidant, a light stabilizer, carbon black, an organic-inorganic composite modifier, a surfactant, a compatilizer, a catalyst and a rheology modifier. The high carbon black photo-oxidative aging resistant silane crosslinked polyethylene insulating material and the preparation method adopt an organic-inorganic composite modifier and a surfactant to carry out modification treatment on carbon black, and form multi-level stable chemical bond connection under the action of a compatilizer, so that the carbon black can be uniformly dispersed in matrix resin and well compatible, the photo-oxidative aging resistant performance is ensured to meet the requirements by a stable material structure, meanwhile, the cracking resistant performance is excellent, the extruded surface of the overhead cable produced by the material is smooth and fine, the tracking resistant performance meets the requirements, and the long-term safe and stable operation of the overhead cable is ensured.
Description
Technical field:
the invention relates to the technical field of cable materials, in particular to a high carbon black photo-oxidative aging resistant silane crosslinked polyethylene insulating material and a preparation method thereof.
The background technology is as follows:
for outdoor overhead insulated cables, the use environment is various, and the outdoor overhead insulated cables are easy to undergo photo-oxidative aging under climatic conditions such as air, rainwater, light irradiation and the like for a long time, so that the damage of an insulating layer structure is caused, the use safety and the service life of the cables can be seriously influenced, and even an insulating cracking phenomenon occurs, so that accidents occur. In addition, when the cable transmits high voltage, a larger current can generate conductor temperature rise, the temperature rise can be conducted to the insulating layer, the electrical insulation of the material can be affected, the tracking phenomenon of the cable insulation is caused, and the tracking can be extinguished in the initial stage. Aiming at the problems, the ultraviolet resistant agent and the carbon black are used for modifying the crosslinked polyethylene in the industry to meet the requirement of photo-oxidative aging resistance, but in an actual material system, the carbon black is added into a high polymer matrix in a particle state, is difficult to disperse well under the condition of more than 2 percent of addition amount, and has the problem of no organic compatibility with the matrix, and at the moment, the carbon black is similar to impurities, and can influence the mechanical strength and the electrical strength of an insulating layer, so that the risks of mechanical cracking, breakdown and the like of a cable are brought.
Further, enterprises improve the compatibility problem with matrix resin by using a coupling agent to carry out surface treatment on carbon black, but under the common adding process, even if the coupling agent is fully treated, the coupling agent is in a physical coating state and lacks chemical bond connection, so that the carbon black subjected to surface treatment cannot be well dispersed and organically compatible, and the problems of inconsistent performance and uneven actual weather resistance can occur. In addition, the extrusion performance can be influenced by adding more carbon black, so that the extrusion surface of the cable is not smooth, and the normal use can be seriously influenced by bulges.
The invention comprises the following steps:
the modification method of the powder is generally carried out by inorganic modification using an acid, a salt or the like, or organic modification using an organic salt, a coupling agent or the like. The carbon black is pretreated by a special modification method, and is comprehensively modified by using an organic-inorganic composite modifier and a compatible modifier, so that the dispersion problem of more carbon black after being added can be effectively solved, the carbon black and a matrix can form stable chemical bond connection, the material structure is stable, the excellent photo-oxidative aging resistance effect is achieved, and the requirements of tracking resistance are met.
The organic-inorganic composite modifier is compounded with organic quaternary ammonium salt, inorganic zinc salt, calcium salt, etc. and the compatilizer is maleic anhydride grafted polyethylene, maleic anhydride grafted metallocene polyethylene or maleic anhydride grafted block copolymer. In the process of modifying and preprocessing the carbon black, the organic-inorganic composite modifier can be attached to the surface of the carbon black to form various bond connections, and under the action of the compatilizer, stable chemical bonds can be further established with matrix resin, so that carbon black particles and the matrix resin are well compatible, and meanwhile, the carbon black is uniformly dispersed, the influence on the material structure after more carbon black is added is solved, the material is free of cracking risk in the use process, and the surface is finer.
The invention provides a high carbon black photo-oxidative aging resistant silane crosslinked polyethylene insulating material, which is a weather-resistant insulating material product developed based on a one-step silane crosslinked polyethylene insulating material process and is prepared from the following raw materials in parts by weight:
wherein the melt flow rate (190 ℃,2.16 kg) of the linear low density polyethylene resin A is 1.8-3.5g/10min; the melt flow rate (190 ℃ C., 2.16 kg) of the linear low-density polyethylene resin B is 18-21g/10min; the high pressure low density polyethylene melt flow rate (190 ℃,2.16 kg) is 1.7-2.6g/10min;
the silane coupling agent is vinyl trimethoxy silane coupling agent;
the initiator is dicumyl peroxide;
the light stabilizer is a hindered amine light stabilizer;
the antioxidant is one or a combination of more of tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester, 4 '-thiobis (6-tert-butyl-3-methylphenol) and N, N' -bis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl ] hydrazine;
the organic-inorganic composite modifier is composed of one of octadecyl quaternary ammonium salt, dioctadecyl benzyl quaternary ammonium salt and hexadecyl trimethyl ammonium bromide and one of zinc stearate, barium stearate, nano calcium carbonate and magnesium hydroxide;
the surfactant is one of vinyl triethoxysilane, vinyl tri (beta-methoxyethoxy) silane and titanate coupling agent;
the compatilizer is one of maleic anhydride grafted polyethylene and maleic anhydride grafted metallocene polyethylene;
the catalyst is dibutyl tin dilaurate;
the rheology modifier is one of fluorine-containing polymer, polyethylene wax and siloxane master batch.
The preparation method of the high carbon black photo-aging resistant silane crosslinked polyethylene insulating material comprises the following steps:
(1) Modifying the carbon black to prepare carbon black modified master batch;
adding carbon black, a light stabilizer and an organic-inorganic composite modifier into a high-speed mixer in proportion, adding a surfactant after starting mixing, mixing at a high speed for 2-5 minutes, adding high-pressure low-density polyethylene, a rheological agent, a compatilizer and a catalyst, mixing for 1-2 minutes, adding a mixed material into a 65 double-screw extruder, mixing and plasticizing the material, cooling the plasticized material by a die orifice brace, drying by water, granulating, and then blowing and drying by a fluidized bed, thereby preparing carbon black modified master batch, wherein the 65 double-screw extruder comprises the following processing steps: one zone 135+ -5deg.C; the second region is 145+/-5 ℃; 155+ -5 ℃ in the third region; four zone 165±5 ℃; five to nine zones 170 + -5 deg.c; ten zone 165±5 ℃; eleven zone 160±5 ℃; the temperature of the machine head is 160+/-5 ℃;
(2) Adding the linear low-density polyethylene resin A, the linear low-density polyethylene resin B, the antioxidant and the carbon black modified master batch into a reciprocating extruder for mixing through weighing ingredients of a weightless type metering scale, extruding and granulating a mixed plasticizing dough through a single screw, and dehydrating and subsequently drying through a centrifugal dehydrator to obtain carbon black pre-dispersed resin particles; the processing temperatures of the reciprocating extruder set are shown in the following table
(3) Heating and drying the prepared carbon black pre-dispersed resin particles, and using a shaking tank, wherein the heating temperature is 60-70 ℃ and the drying time is 1-2 hours;
(4) Adding the dried carbon black pre-dispersed resin particles into a shaking tank, preheating and drying for 30-60 minutes at the preheating temperature of 60-70 ℃, adding the compound silane coupling agent, and fully mixing in the shaking tank for 1-2 hours to obtain a finished product.
The beneficial effects of the invention are as follows: the high carbon black photo-oxidative aging resistant silane crosslinked polyethylene insulating material and the preparation method adopt an organic-inorganic composite modifier and a surfactant to carry out modification treatment on carbon black, and are connected with chemical bonds forming multi-level stability under the action of a compatilizer, so that the carbon black can be uniformly dispersed in matrix resin and well compatible with the chemical bonds, the photo-oxidative aging resistant performance of the material is ensured to meet the requirements by a stable structure, meanwhile, the cracking resistant performance is excellent, the extruded surface of the overhead cable produced by the material is smooth and fine, the tracking resistant performance meets the requirements, and the long-term safe and stable operation of the overhead cable is ensured.
The specific embodiment is as follows:
the following detailed description of the preferred embodiments of the invention will provide those skilled in the art with a better understanding of the invention with its advantages and features, and thus define the scope of the invention more clearly and clearly.
As shown in FIG. 1, the invention provides a preparation method of a high carbon black photo-oxidative aging resistant silane crosslinked polyethylene insulating material, which comprises the following steps:
(1) Modifying the carbon black to prepare carbon black modified master batch;
adding carbon black, a light stabilizer and an organic-inorganic composite modifier into a high-speed mixer in proportion, adding a surfactant after starting mixing, mixing at a high speed for 2-5 minutes, adding high-pressure low-density polyethylene, a rheological agent, a compatilizer and a catalyst, mixing for 1-2 minutes, adding a mixed material into a 65 double-screw extruder, mixing and plasticizing the material, cooling the plasticized material by a die orifice brace, drying by water, granulating, and then blowing and drying by a fluidized bed, thereby preparing carbon black modified master batch, wherein the 65 double-screw extruder comprises the following processing steps: one zone 135+ -5deg.C; the second region is 145+/-5 ℃; 155+ -5 ℃ in the third region; four zone 165±5 ℃; five to nine zones 170 + -5 deg.c; ten zone 165±5 ℃; eleven zone 160±5 ℃; the temperature of the machine head is 160+/-5 ℃;
(2) Adding the linear low-density polyethylene resin A, the linear low-density polyethylene resin B, the antioxidant and the carbon black modified master batch into a reciprocating extruder for mixing through weighing ingredients of a weightless type metering scale, extruding and granulating a mixed plasticizing dough through a single screw, and dehydrating and subsequently drying through a centrifugal dehydrator to obtain carbon black pre-dispersed resin particles; the processing temperatures of the reciprocating extruder set are shown in the following table
(3) Heating and drying the prepared carbon black pre-dispersed resin particles, and using a shaking tank, wherein the heating temperature is 60-70 ℃ and the drying time is 1-2 hours;
(4) Adding the dried carbon black pre-dispersed resin particles into a shaking tank, preheating and drying for 30-60 minutes at the preheating temperature of 60-70 ℃, adding the compound silane coupling agent, and fully mixing in the shaking tank for 1-2 hours to obtain a finished product.
Examples 1 and 2 of the present invention are shown in the following table:
| material name | Example 1 | Example 2 |
| Sea-land petrochemical LLDPE7042 | 70 | 70 |
| Marine land petrochemical LLDPEM2320 | 15 | 15 |
| Shanghai petrochemical DJ200A | 5 | 5 |
| Silane A171 | 1.4 | 1.4 |
| Dicumyl peroxide | 0.08 | 0.08 |
| Antioxidant 1010 | 0.15 | 0.15 |
| Antioxidant 1024 | 0.15 | 0.15 |
| Light stabilizer 770DF | 0.2 | 0.2 |
| Carbon black N550 | 2.5 | 4 |
| Octadecyl quaternary ammonium salt | 0.4 | 0.6 |
| Zinc stearate | 0.4 | 0.6 |
| Silane coupling agent A151 | 0.02 | 0.04 |
| Compatibilizer MC226 | 1 | 1.5 |
| Dibutyl tin dilaurate | 0.05 | 0.05 |
| PPA5924 | 3 | 3 |
Comparative examples are shown in the following table:
the test data for the examples of the invention and the comparative examples are shown in the following table:
the test performance data and the extrusion test observe that the extrusion surfaces of the embodiment 1 and the embodiment 2 are smooth and fine, the data stability is good, especially the artificial weather aging performance test data are very ideal, the photo-oxidative aging resistance is excellent, and the subsequent preparation test piece passes through the GB/T6553-2014 standard 5.2 method I: constant tracking voltage method 1A4.5 (4.5 kv/6 h) test.
Comparative examples 1-1 and 2-1 were organic modified with only ammonium salt and surfactant, and the artificial weathering data was poor from the comparative data, and when the carbon black addition was 4%, the extrusion surface was long and the environmental stress crack resistance test was not passed; comparative examples 1-2 and 2-2 are carbon blacks modified with an inorganic modifier and a surfactant, and the data of the artificial weathering data are worse from the comparative data, and at an addition of 4% of carbon black, the extrusion appears to be significantly small particles, and the environmental stress crack resistance test is failed. The modified carbon black in the two modification modes has no stable chemical bond connection with the matrix resin, and has obvious degradation of performance under the simulated photo-oxidative aging effect, and is unqualified.
The comparative examples 1-3 and 2-3 were compared with the examples minus the addition of the surfactant, the organic-inorganic composite modifier modified the carbon black, and under the action of the compatibilizer, multiple bond connections were established between the carbon black and the organic-inorganic composite modifier, and the test data were examined for acceptable artificial weathering, but the aging data were compared with the aging data for 42 days and 21 days, the phenomenon of approaching the standard line occurred, and the surface structure stability was somewhat impaired under the long-term aging. The extruded surface was also observed to be rough at a carbon black level of 4% for comparative examples 2-3. Comparative examples 1-4 and 2-4 were free of compatibilizers, deviation of the data from artificial weathering, and environmental stress crack resistance of comparative examples 2-4 with 4% carbon black added were not yet tested.
As can be seen from comprehensive data, the embodiment of the invention adopts the organic-inorganic composite modifier and the surfactant to modify the carbon black, and is connected with the chemical bonds forming multi-level stability under the action of the compatilizer, so that the carbon black can be uniformly dispersed and well compatible in matrix resin, and the stable structure of the material ensures that the photo-oxidative aging resistance meets the requirements and has excellent cracking resistance. The extruded surface of the overhead cable produced by using the material is smooth and fine, the tracking resistance meets the requirements, and the long-term safe and stable operation of the overhead cable is ensured.
Finally, it should be noted that: the above embodiments are only for illustrating the present invention and not for limiting the technical solution described in the present invention; thus, while the invention has been described in detail with reference to the various embodiments described above, it will be understood by those skilled in the art that the invention may be modified or equivalents; all technical solutions and modifications thereof that do not depart from the spirit and scope of the present invention are intended to be included in the scope of the appended claims.
Claims (10)
1. The high carbon black photo-aging resistant silane crosslinked polyethylene insulating material is characterized by being prepared from the following raw materials in parts by weight:
the linear low-density polyethylene resin A is a Zhenhai petrochemical LLDPE7042, and the linear low-density polyethylene resin B is a Zhenhai petrochemical LLDPE M2320.
2. The high carbon black photo-aging resistant silane crosslinked polyethylene insulation according to claim 1, wherein the linear low density polyethylene resin a melt flow rate is 1.8-3.5g/10min at 190 ℃,2.16 kg; the melt flow rate of the linear low density polyethylene resin B is 18-21g/10min at 190 ℃ and 2.16 kg; the high pressure low density polyethylene melt flow rate is 1.7-2.6g/10min at 190 ℃ and 2.16 kg.
3. The high carbon black photo-aging resistant silane crosslinked polyethylene insulation material according to claim 1, wherein the silane coupling agent is a vinyl trimethoxy silane coupling agent; the initiator is dicumyl peroxide; the light stabilizer is a hindered amine light stabilizer.
4. The high carbon black photo-aging resistant silane crosslinked polyethylene insulation according to claim 1, wherein the antioxidant is one or more of pentaerythritol tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], 4 '-thiobis (6-tert-butyl-3-methylphenol), N' -bis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl ] hydrazine.
5. The high carbon black photo-aging resistant silane crosslinked polyethylene insulation material according to claim 1, wherein the organic-inorganic composite modifier is composed of one of octadecyl quaternary ammonium salt, dioctadecyl benzyl quaternary ammonium salt and hexadecyl trimethyl ammonium bromide and one of zinc stearate, barium stearate, nano calcium carbonate and magnesium hydroxide.
6. The high carbon black photo-aging resistant silane crosslinked polyethylene insulation material according to claim 1, wherein the surfactant is one of vinyltriethoxysilane, vinyltris (beta-methoxyethoxy) silane, and titanate coupling agent.
7. The high carbon black photo-aging resistant silane crosslinked polyethylene insulation material according to claim 1, wherein the compatibilizer is one of maleic anhydride grafted polyethylene and maleic anhydride grafted metallocene polyethylene.
8. The high carbon black photo-aging resistant silane crosslinked polyethylene insulation according to claim 1, wherein the catalyst is dibutyl tin dilaurate.
9. The high carbon black photo-aging resistant silane crosslinked polyethylene insulation of claim 1, wherein the rheology modifier is one of a fluoropolymer, a polyethylene wax, a silicone masterbatch.
10. A method for preparing the high carbon black photo-aging resistant silane crosslinked polyethylene insulation material according to any one of claims 1-9, comprising the steps of:
(1) Modifying the carbon black to prepare carbon black modified master batch;
adding carbon black, a light stabilizer and an organic-inorganic composite modifier into a high-speed mixer in proportion, adding a surfactant after starting mixing, mixing at a high speed for 2-5 minutes, adding high-pressure low-density polyethylene, a rheological agent, a compatilizer and a catalyst, mixing for 1-2 minutes, adding a mixed material into a 65 double-screw extruder, mixing and plasticizing the material, cooling the plasticized material by a die orifice brace, drying by water, granulating, and then blowing and drying by a fluidized bed, thereby preparing carbon black modified master batch, wherein the 65 double-screw extruder comprises the following processing steps: one zone 135+ -5deg.C; the second region is 145+/-5 ℃; 155+ -5 ℃ in the third region; four zone 165±5 ℃; five to nine zones 170 + -5 deg.c; ten zone 165±5 ℃; eleven zone 160±5 ℃; the temperature of the machine head is 160+/-5 ℃;
(2) Adding the linear low-density polyethylene resin A, the linear low-density polyethylene resin B, the antioxidant and the carbon black modified master batch into a reciprocating extruder for mixing through weighing ingredients of a weightless type metering scale, extruding and granulating a mixed plasticizing dough through a single screw, and dehydrating and subsequently drying through a centrifugal dehydrator to obtain carbon black pre-dispersed resin particles; the processing temperature of the reciprocating extrusion unit is
And (3) an upper stage machine: one zone 140 + -5 ℃; the second region is 160+/-5 ℃; three zone 165±5 ℃; four regions 170+ -5deg.C; five zones 165±5 ℃;
lower machine: one zone 140 + -5 ℃; 155+ -5 ℃ in the second region; 155+ -5 ℃ in the third region; the temperature of the machine head is 150+/-5 ℃;
(3) Heating and drying the prepared carbon black pre-dispersed resin particles at the heating temperature of 60-70 ℃ for 1-2 hours;
(4) Adding the dried carbon black pre-dispersed resin particles into a shaking tank, preheating and drying for 30-60 minutes at the preheating temperature of 60-70 ℃, adding the compound silane coupling agent, and fully mixing in the shaking tank for 1-2 hours to obtain a finished product.
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Denomination of invention: High carbon black, photo oxidative aging resistant, silane crosslinked polyethylene insulation material and preparation method Granted publication date: 20230623 Pledgee: China Postal Savings Bank Co.,Ltd. Nanjing Gaochun Branch Pledgor: NANJING ZHONGCHAO NEW MATERIALS Corp. Registration number: Y2024980002363 |
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