CN103435897A - Microwave induced intumescent flame-retardant silane crosslinked polyolefin sheath material for cables and preparation method thereof - Google Patents
Microwave induced intumescent flame-retardant silane crosslinked polyolefin sheath material for cables and preparation method thereof Download PDFInfo
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- CN103435897A CN103435897A CN2013104216119A CN201310421611A CN103435897A CN 103435897 A CN103435897 A CN 103435897A CN 2013104216119 A CN2013104216119 A CN 2013104216119A CN 201310421611 A CN201310421611 A CN 201310421611A CN 103435897 A CN103435897 A CN 103435897A
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Abstract
The invention relates to a sheath material and a preparation method thereof and provides a microwave induced intumescent flame-retardant silane crosslinked polyolefin sheath material for cables and a preparation method thereof for solving such technical problems in the existing preparation method of flame-retardant silane crosslinked sheath materials as long-time boiling with water is required, the stability and flame retardant effect of the product are poor. The material is prepared from a polyolefin resin, an intumescent flame retardant, a silane coupling agent, a microwave absorbent, a water bringing agent, a polyfunctional group crosslinking agent, a crosslinking accelerant and an antioxidant. The preparation method comprises the steps of carrying out melt mixing on the polyolefin resin, the intumescent flame retardant, the silane coupling agent, the microwave absorbent, the water bringing agent, the polyfunctional group crosslinking agent, the crosslinking accelerant and the antioxidant, carrying out granulation and tabletting, then carrying out microwave induced crosslinking and putting the product at room temperature, thus preparing the material. The mechanical property of the material prepared by the preparation method is obviously increased, the tensile strength is improved by nearly 20% and the oxygen index is improved by more than 70%. The material and the preparation method belong to the field of preparation of polyolefin sheath materials.
Description
Technical field
The present invention relates to a kind of sheath material and preparation method thereof.
Background technology
All many-sided excellent properties such as the processibility that tensile strength is high, impelling strength good owing to having for flame retardant polyolefine material, wear-resisting, self lubricity, electric property are good, good and flame retardant resistance, be widely used in the fields such as electronics, electrical equipment, automobile, machinofacture, chemical industry, food, daily necessities, health care at present.But, in the cable material Application Areas, the performance of flame retardant polyolefine material can't meet the requirement in practical application fully.For example, the aspects such as the intensity of common polyolefine material, heat-drawn wire and solvent resistance can't reach the requirement under some particular service requirement.For the above shortcoming of flame retardant polyolefine material, crosslinked is a kind of effective terms of settlement.Crosslinkedly can form three-dimensional network structure, can improve on the one hand intensity, resistance toheat and the heat-drawn wire of material, limited on the other hand the water-intake rate of polyolefine material under wet environment and improved its solvent resistance.Make at present the crosslinked existing preparation method of flame retardant polyolefine material mainly contain chemical crosslink technique, crosslinking electron beam irradiation method and crosslinked with silicane.Existing research shows that a lot of materials have special sorption for microwave, under the effect of microwave, molecule can heat up rapidly, understand the molecule that decomposition reaction or inducing peripheral occur self corresponding decomposition reaction (Journal of Chemical Industry and Engineering 2006,57,663) occurs when temperature acquires a certain degree.Therefore, in the silane crosslinked insulating material system, introducing microwave absorbing material and fire retardant can be at microwave induced lower generation moment high temperature, can decompose if exist in system the molecule that produces water, system both can produce after microwave induced and have the crosslinked internal water molecule of catalysis silane molecule.
Chemically crosslinked need to be reacted for a long time in High Temperature High Pressure and specific equipment, and energy expenditure is large, and production efficiency is low; And, because most of polyolefinic melt temperatures are higher, peroxide initiator can decompose in advance, causes precrosslink.And the investment of high-energy radiation cross-linking apparatus is high, Operation and Maintenance is complicated, requirement of shelter is harsh, product cost is high, and the high-energy radiation energy is higher simultaneously, can cause the fracture of nylon molecular backbone chain, also can cause the deterioration to material internal structural damage and correlated performance.Crosslinked with silicane is to utilize silane to pass through fusion-grafting, receives on macromolecular chain, and then side group is hydrolyzed, and dehydrating condensation under catalyzer exists, form Si-O-Si crosslinked, but need poach when crosslinked, expends man-hour long, and product stability is poor.
Summary of the invention
The objective of the invention is needs poach in order to solve the flame-proof silicone hydride crosslinked sheath material of existing preparation, and the poach time is long, the technical problem that product stability is poor, flame retardant effect is poor, provide a kind of microwave induced expandable flame retardant silanes crosslinked cable polyolefin jacket material and preparation method thereof.
Microwave induced expandable flame retardant silanes crosslinked cable is made by the polyolefin resin of 100 parts of dryings, 25～80 parts of expansion type flame retardants, 0.1～4 part of silane coupling agent, 0.2～3 part of microwave absorption, 0.1～4 part of product aqua, 0.3～5 part of multi-group crosslink agent, 0.01～5 part of crosslinking accelerator and 0.07～0.5 part of oxidation inhibitor by weight with the polyolefin jacket material.
Described polyolefin resin is a kind of in high density polyethylene(HDPE) (HDPE), medium-density polyethylene (MDPE), Low Density Polyethylene (LDPE), low density linear polyethylene (LLDPE), ethylene-vinyl acetate copolymer (EVA) and polyolefin elastomer or wherein several combination.
Described expansion type flame retardant is a kind of in expansion type flame retardant IFR-P500, expansion type flame retardant IFR-P601, expansion type flame retardant IFR-P602, expansion type flame retardant IFR-P603, expansion type flame retardant IFR-T800 and expansion type flame retardant IFR-MT800 or wherein several combination.
Described microwave absorption is a kind of in carbon black, graphite, Manganse Dioxide and barium ferrite or wherein several combination.
Described product aqua is magnesium hydroxide (Mg (OH)
2), aluminium hydroxide (Al (OH)
3), zinc borate (2ZnOB
2o
33.5H
2o) and Cadmium sulfate hydrate (CdSO
48H
2o) a kind of in or wherein several combination.
Described silane coupling agent is vinyltrimethoxy silane (A171), vinyltriethoxysilane (A151), a kind of in γ aminopropyltriethoxy silane, benzene n-formyl sarcolysine ethyl triethoxy silicane alkane, γ-second phenodiazine base propyl trimethoxy silicane, β-(3,4-epoxycyclohexyl) ethyl trimethoxy silane and γ-propyl methacrylate base Trimethoxy silane or wherein several combination.
Described multi-group crosslink agent is a kind of in triallyl cyanurate (TAC), cyamelide triallyl (TAIC), trimethylolpropane tris (methyl) acrylate (TMPTA), trimethylolpropane tris allyl ether (TMPAE), tetramethylolmethane three allyl ethers (PETAE), tetramethylolmethane tetraene propyl ether and triglycol methacrylic ester (TEGMA) or wherein several combination.
Described crosslinking accelerator is ethylene-tetrafluoroethylene copolymer, ethene-1, a kind of in chlorotrifluoroethylcopolymer copolymer, ethene-fluoride copolymers, hexachloroethane and tetrachloromethane or wherein several combination.
Described oxidation inhibitor is phenolic antioxidant, phosphite ester kind antioxidant, phosphoric acid ester oxidation inhibitor and the mixture that contains two or more composition in the thioesters kind antioxidant;
Described phenolic antioxidant is 2,6-di-tert-butylphenol, 2,4,6-tri-tert-butylphenol (oxidation inhibitor 246), 4,4 '-thiobis (6-tertiary butyl-3-methylphenol) (antioxidant 300) or four [methylene radical-3-(3 ', 5 '-di-tert-butyl-4 '-hydroxy phenyl) propionic acid] pentaerythritol ester (antioxidant 1010);
Described phosphite ester kind antioxidant is triphenyl phosphite (TPP), tricresyl phosphite (2,4-di-tert-butyl phenyl) ester (irgasfos 168) or the different monooctyl ester of tricresyl phosphite (TIOP);
Described phosphoric acid ester oxidation inhibitor is the tricresyl phosphate benzene methyl;
Described is Tyox B (DLTP), thio-2 acid bay octadecyl ester (LSTP) or thio-2 acid two (13) ester (DTDTP) containing the thioesters kind antioxidant.
Microwave induced expandable flame retardant silanes crosslinked cable is as follows by the preparation method of polyolefin jacket material:
One, take by weight 100 parts of polyolefin resines 80 ℃～120 ℃ of dryings, 25～80 parts of expansion type flame retardants, 0.1～4 part of silane coupling agent, 0.2～3 part of microwave absorption, 0.1～4 part of product aqua, 0.3～5 part of multi-group crosslink agent, 0.01～5 part of crosslinking accelerator and 0.07～0.5 part of oxidation inhibitor;
Two, at 160 ℃～200 ℃, polyolefin resin, expansion type flame retardant, silane coupling agent, microwave absorption, product aqua, multi-group crosslink agent, crosslinking accelerator and oxidation inhibitor are carried out to melting mixing 5min, then by the twin screw extruder granulation of 190 ℃～210 ℃, obtain the sample particle mixed;
Three, the sample particle of mixing is placed in to the vulcanizer compressing tablet, and then be microwave induced crosslinked 40s～80s under 2450MHz, the power condition that is 650W-～1000W in frequency, place 16 hours in room temperature, obtain microwave induced expandable flame retardant silanes crosslinked cable polyolefin jacket material.
The present invention has the following advantages:
One, the microwave induced expandable flame retardant silanes crosslinked cable that prepared by the present invention with the polyolefin jacket material, can reduce produce power consumption, do not need poach, environment friendly and pollution-free, cost is low, product is high temperature resistant, flame retardant properties is good;
Two, the microwave induced expandable flame retardant silanes crosslinked cable that prepared by the present invention is good with the polyolefin jacket material property, has excellent resistance toheat, water resistance and flame retardant properties, and application prospect is extensive;
Three, the microwave induced expandable flame retardant silanes crosslinked cable that prepared by the present invention is low with the investment of polyolefin jacket material installation, and simple, easy to operate, the easy protection of technique, cost are low, realistic need of production;
Four, the microwave induced expandable flame retardant silanes crosslinked cable that prepared by the present invention obviously increases by the polyolefin jacket mechanics of materials, and tensile strength has nearly improved 20%, and oxygen index improves more than 70%, and the water tolerance performance is greatly improved.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: the microwave induced expandable flame retardant silanes crosslinked cable of present embodiment is made by the polyolefin resin of 100 parts of dryings, 25～80 parts of expansion type flame retardants, 0.1～4 part of silane coupling agent, 0.2～3 part of microwave absorption, 0.1～4 part of product aqua, 0.3～5 part of multi-group crosslink agent, 0.01～5 part of crosslinking accelerator and 0.07～0.5 part of oxidation inhibitor by weight with the polyolefin jacket material.
Embodiment two: present embodiment is different from embodiment one is that described polyolefin resin is a kind of in high density polyethylene(HDPE), medium-density polyethylene, Low Density Polyethylene, low density linear polyethylene, ethylene-vinyl acetate copolymer and polyolefin elastomer or wherein several combination.Other is identical with embodiment one.
When the polyolefin resin described in present embodiment is composition, between each composition, be arbitrarily than.
Embodiment three: present embodiment is different from one of embodiment one or two is that described expansion type flame retardant is a kind of in expansion type flame retardant IFR-P500, expansion type flame retardant IFR-P601, expansion type flame retardant IFR-P602, expansion type flame retardant IFR-P603, expansion type flame retardant IFR-T800 and expansion type flame retardant IFR-MT800 or wherein several combination.Other is not identical with one of embodiment one or two.
When the expansion type flame retardant described in present embodiment is composition, between each composition, be arbitrarily than.
Expansion type flame retardant IFR-P500 described in present embodiment, expansion type flame retardant IFR-P601, expansion type flame retardant IFR-P602, expansion type flame retardant IFR-P603, expansion type flame retardant IFR-T800 and expansion type flame retardant IFR-MT800 are manufactured by Heilongjiang Province Run Te Science and Technology Ltd..
Embodiment four: present embodiment is different from one of embodiment one to three is that described microwave absorption is a kind of in carbon black, graphite, Manganse Dioxide and barium ferrite or wherein several combination.Other is identical with one of embodiment one to three.
When the microwave absorption described in present embodiment is composition, between each composition, be arbitrarily than.
Embodiment five: present embodiment is different from one of embodiment one to four is that described product aqua is a kind of in magnesium hydroxide, aluminium hydroxide, zinc borate and Cadmium sulfate hydrate or wherein several combination.Other is identical with one of embodiment one to four.
When the product aqua described in present embodiment is composition, between each composition, be arbitrarily than.
Embodiment six: what present embodiment was different from one of embodiment one to five is that described silane coupling agent is vinyltrimethoxy silane, vinyltriethoxysilane, a kind of in γ aminopropyltriethoxy silane, benzene n-formyl sarcolysine ethyl triethoxy silicane alkane, γ-second phenodiazine base propyl trimethoxy silicane, β-(3,4-epoxycyclohexyl) ethyl trimethoxy silane and γ-propyl methacrylate base Trimethoxy silane or wherein several combination.Other is identical with one of embodiment one to five.
When the silane coupling agent described in present embodiment is composition, between each composition, be arbitrarily than.
Embodiment seven: present embodiment is different from one of embodiment one to six is that described multi-group crosslink agent is a kind of in triallyl cyanurate, cyamelide triallyl, trimethylolpropane tris (methyl) acrylate, trimethylolpropane tris allyl ether, tetramethylolmethane three allyl ethers, tetramethylolmethane tetraene propyl ether and triglycol methacrylic ester or wherein several combination.Other is identical with one of embodiment one to six.
When the multi-group crosslink agent described in present embodiment is composition, between each composition, be arbitrarily than.
Embodiment eight: what present embodiment was different from one of embodiment one to seven is that described crosslinking accelerator is ethylene-tetrafluoroethylene copolymer, ethene-1, a kind of in chlorotrifluoroethylcopolymer copolymer, ethene-fluoride copolymers, hexachloroethane and tetrachloromethane or wherein several combination.Other is identical with one of embodiment one to seven.
When the crosslinking accelerator described in present embodiment is composition, between each composition, be arbitrarily than.
Embodiment nine: what present embodiment was different from one of embodiment one to eight is that described oxidation inhibitor is phenolic antioxidant, phosphite ester kind antioxidant, phosphoric acid ester oxidation inhibitor and the mixture that contains two or more composition in the thioesters kind antioxidant;
Described phenolic antioxidant is 2,6-di-tert-butylphenol, 2,4,6-tri-tert-butylphenol, 4,4 '-thiobis (6-tertiary butyl-3-methylphenol) or four [methylene radical-3-(3 ', 5 '-di-tert-butyl-4 '-hydroxy phenyl) propionic acid] pentaerythritol ester;
Described phosphite ester kind antioxidant is triphenyl phosphite, tricresyl phosphite (2,4-di-tert-butyl phenyl) ester or the different monooctyl ester of tricresyl phosphite;
Described phosphoric acid ester oxidation inhibitor is the tricresyl phosphate benzene methyl;
Described is Tyox B, thio-2 acid bay octadecyl ester or thio-2 acid two (13) ester containing the thioesters kind antioxidant.Other is identical with one of embodiment one to eight.
When the oxidation inhibitor described in present embodiment is composition, between each composition, be arbitrarily than.
Embodiment ten: the described microwave induced expandable flame retardant silanes crosslinked cable of embodiment one is as follows by the preparation method of polyolefin jacket material:
One, take by weight 100 parts of polyolefin resines 80 ℃～120 ℃ of dryings, 25～80 parts of expansion type flame retardants, 0.1～4 part of silane coupling agent, 0.2～3 part of microwave absorption, 0.1～4 part of product aqua, 0.3～5 part of multi-group crosslink agent, 0.01～5 part of crosslinking accelerator and 0.07～0.5 part of oxidation inhibitor;
Two, at 160 ℃～200 ℃, polyolefin resin, expansion type flame retardant, silane coupling agent, microwave absorption, product aqua, multi-group crosslink agent, crosslinking accelerator and oxidation inhibitor are carried out to melting mixing 5min, then by the twin screw extruder granulation of 190 ℃～210 ℃, obtain the sample particle mixed;
Three, the sample particle of mixing is placed in to the vulcanizer compressing tablet, and then be microwave induced crosslinked 40s～80s under 2450MHz, the power condition that is 650W～1000W in frequency, place 16 hours in room temperature, obtain microwave induced expandable flame retardant silanes crosslinked cable polyolefin jacket material.
Described polyolefin resin is a kind of in high density polyethylene(HDPE) (HDPE), medium-density polyethylene (MDPE), Low Density Polyethylene (LDPE), low density linear polyethylene (LLDPE), ethylene-vinyl acetate copolymer (EVA) and polyolefin elastomer or wherein several combination.
Is described expansion type flame retardant that these models of IFR-P500, IFR-P601, IFR-P602, IFR-P603, IFR-T800 and IFR-MT800(are known?) in a kind of or wherein several combination.
Described microwave absorption is a kind of in carbon black, graphite, Manganse Dioxide and barium ferrite or wherein several combination.
Described product aqua is magnesium hydroxide (Mg (OH)
2), aluminium hydroxide (Al (OH)
3), zinc borate (2ZnOB
2o
33.5H
2o) and Cadmium sulfate hydrate (CdSO
48H
2o) a kind of in or wherein several combination.
Described silane coupling agent is vinyltrimethoxy silane (A171), vinyltriethoxysilane (A151), a kind of in γ aminopropyltriethoxy silane, benzene n-formyl sarcolysine ethyl triethoxy silicane alkane, γ-second phenodiazine base propyl trimethoxy silicane, β-(3,4-epoxycyclohexyl) ethyl trimethoxy silane and γ-propyl methacrylate base Trimethoxy silane or wherein several combination.
Described multi-group crosslink agent is a kind of in triallyl cyanurate (TAC), cyamelide triallyl (TAIC), trimethylolpropane tris (methyl) acrylate (TMPTA), trimethylolpropane tris allyl ether (TMPAE), tetramethylolmethane three allyl ethers (PETAE), tetramethylolmethane tetraene propyl ether and triglycol methacrylic ester (TEGMA) or wherein several combination.
Described crosslinking accelerator is ethylene-tetrafluoroethylene copolymer, ethene-1, a kind of in chlorotrifluoroethylcopolymer copolymer, ethene-fluoride copolymers, hexachloroethane and tetrachloromethane or wherein several combination.
Described oxidation inhibitor is phenolic antioxidant, phosphite ester kind antioxidant, phosphoric acid ester oxidation inhibitor and the mixture that contains two or more composition in the thioesters kind antioxidant;
Described phenolic antioxidant is 2,6-di-tert-butylphenol, 2,4,6-tri-tert-butylphenol (oxidation inhibitor 246), 4,4 '-thiobis (6-tertiary butyl-3-methylphenol) (antioxidant 300) or four [methylene radical-3-(3 ', 5 '-di-tert-butyl-4 '-hydroxy phenyl) propionic acid] pentaerythritol ester (antioxidant 1010);
Described phosphite ester kind antioxidant is triphenyl phosphite (TPP), tricresyl phosphite (2,4-di-tert-butyl phenyl) ester (irgasfos 168) or the different monooctyl ester of tricresyl phosphite (TIOP);
Described phosphoric acid ester oxidation inhibitor is the tricresyl phosphate benzene methyl;
Described is Tyox B (DLTP), thio-2 acid bay octadecyl ester (LSTP) or thio-2 acid two (13) ester (DTDTP) containing the thioesters kind antioxidant.
Microwave induced expandable flame retardant silanes crosslinked cable prepared by present embodiment obviously increases by the polyolefin jacket mechanics of materials, and tensile strength has nearly improved 20%, and heat-drawn wire improves 20-30%, and the water tolerance performance is greatly improved.
Adopt following experimental verification effect of the present invention:
Experiment one:
Microwave induced expandable flame retardant silanes crosslinked cable is as follows by the preparation method of polyolefin jacket material:
One, low density linear polyethylene LLDPE7042, the 28g expansion type flame retardant IFR-P500,0.14g silane coupling A 171,0.21g carbon black, the 0.19g that take the 100g drying produce aqua Mg (OH)
2, 0.42g multi-group crosslink agent TAIC, 0.032g crosslinking accelerator, ethene-fluoride copolymers and 0.19g composite antioxidant, composite antioxidant is comprised of 0.07g antioxidant 1010,0.05g tricresyl phosphate benzene methyl and 0.07g DLTP;
Two, each component taken in step 1 is put into to the Banbury mixer banburying of 160 ℃～200 ℃, melting mixing 5min, then by the twin screw extruder granulation of 190 ℃～210 ℃, obtain the sample particle mixed;
Three, the sample particle of mixing is placed in to the vulcanizer compressing tablet, and then be microwave induced crosslinked 60s under 2450MHz, the power condition that is 800W in frequency, place 16 hours in room temperature, obtain microwave induced expandable flame retardant silanes crosslinked cable polyolefin jacket material.
Experiment two:
Microwave induced expandable flame retardant silanes crosslinked cable is as follows by the preparation method of polyolefin jacket material:
One, low density linear polyethylene LLDPE7066, the 35g expansion type flame retardant IFR-P601,0.6g silane coupling A 171,0.29g graphite, the 0.33g that take the 100g drying produce aqua Al (OH)
3, 4.25g multi-group crosslink agent TMPTA, 0.15g crosslinking accelerator chlorotrifluoroethylcopolymer copolymer and 0.26g composite antioxidant, composite antioxidant is comprised of 0.06g antioxidant 300,0.15g irgasfos 168 and 0.05g DTDTP;
Two, each component taken in step 1 is put into to the Banbury mixer banburying of 160 ℃～200 ℃, melting mixing 5min, then by the twin screw extruder granulation of 190 ℃～210 ℃, obtain the sample particle mixed;
Three, the sample particle of mixing is placed in to the vulcanizer compressing tablet, and then be microwave induced crosslinked 60s under 2450MHz, the power condition that is 800W in frequency, place 16 hours in room temperature, obtain microwave induced expandable flame retardant silanes crosslinked cable polyolefin jacket material.
Experiment three:
Microwave induced expandable flame retardant silanes crosslinked cable is as follows by the preparation method of polyolefin jacket material:
One, take medium-density polyethylene MDPE FB2310,35g expansion type flame retardant IFR-P602,2.5g silane coupling A 151, the 2.5g Manganse Dioxide (MnO of 100g drying
2), 1.9g produces aqua zinc borate, 4.5g multi-group crosslink agent tetramethylolmethane tetraene propyl ether, 1.9g crosslinking accelerator ethylene-tetrafluoroethylene copolymer and 0.35g composite antioxidant, composite antioxidant is by 0.1g oxidation inhibitor 2, and 6-di-tert-butylphenol, 0.15g oxidation inhibitor tricresyl phosphate benzene methyl and 0.1g DLTP form;
Two, each component taken in step 1 is put into to the Banbury mixer banburying of 160 ℃～200 ℃, melting mixing 5min, then by the twin screw extruder granulation of 190 ℃～210 ℃, obtain the sample particle mixed;
Three, the sample particle of mixing is placed in to the vulcanizer compressing tablet, and then be microwave induced crosslinked 60s under 2450MHz, the power condition that is 800W in frequency, place 16 hours in room temperature, obtain microwave induced expandable flame retardant silanes crosslinked cable polyolefin jacket material.
Experiment four:
Microwave induced expandable flame retardant silanes crosslinked cable is as follows by the preparation method of polyolefin jacket material:
One, medium-density polyethylene MDPE3721C, the 48g expansion type flame retardant IFR-P603,1.9g silane coupling A 171,2.6g graphite, the 1.32g that take the 100g drying produce aqua Mg (OH)
2, 3.8g multi-group crosslink agent PETAE, 3.5g crosslinking accelerator hexachloroethane and 0.5g composite antioxidant, composite antioxidant is comprised of 0.25g antioxidant 1010,0.15g oxidation inhibitor TIOP and 0.1g DLTP;
Two, each component taken in step 1 is put into to the Banbury mixer banburying of 160 ℃～200 ℃, melting mixing 5min, then by the twin screw extruder granulation of 190 ℃～210 ℃, obtain the sample particle mixed;
Three, the sample particle of mixing is placed in to the vulcanizer compressing tablet, and then be microwave induced crosslinked 60s under 2450MHz, the power condition that is 800W in frequency, place 16 hours in room temperature, obtain microwave induced expandable flame retardant silanes crosslinked cable polyolefin jacket material.
Experiment five:
Microwave induced expandable flame retardant silanes crosslinked cable is as follows by the preparation method of polyolefin jacket material:
One, high density polyethylene 5000s, the 23g expansion type flame retardant IFR-T800,2.5g silane coupling A 151,1.9g barium ferrite, the 1.8g that take the 100g drying produce aqua Cadmium sulfate hydrate, 3.2g multi-group crosslink agent triglycol methacrylic ester, 2.9g crosslinking accelerator ethene-1 and 0.52g composite antioxidant, and composite antioxidant is comprised of 0.2g oxidation inhibitor 246,0.16g oxidation inhibitor TPP and 0.16g LSTP;
Two, each component taken in step 1 is put into to the Banbury mixer banburying of 160 ℃～200 ℃, melting mixing 5min, then by the twin screw extruder granulation of 190 ℃～210 ℃, obtain the sample particle mixed;
Three, the sample particle of mixing is placed in to the vulcanizer compressing tablet, and then be microwave induced crosslinked 60s under 2450MHz, the power condition that is 800W in frequency, place 16 hours in room temperature, obtain microwave induced expandable flame retardant silanes crosslinked cable polyolefin jacket material.
Experiment six:
Microwave induced expandable flame retardant silanes crosslinked cable is as follows by the preparation method of polyolefin jacket material:
One, high density polyethylene 5300B, the 75g expansion type flame retardant IFR-P601,3.5g silane coupling A 171,1.8g carbon black, the 2.6g that take the 100g drying produce aqua Mg (OH)
2, 3.0g multi-group crosslink agent TMPTA, 4.8g crosslinking accelerator tetrachloromethane and 0.36g composite antioxidant, composite antioxidant is comprised of 0.15g antioxidant 1010,0.09g irgasfos 168 and 0.12g DTDTP;
Two, each component taken in step 1 is put into to the Banbury mixer banburying of 160 ℃～200 ℃, melting mixing 5min, then by the twin screw extruder granulation of 190 ℃～210 ℃, obtain the sample particle mixed;
Three, the sample particle of mixing is placed in to the vulcanizer compressing tablet, and then be microwave induced crosslinked 60s under 2450MHz, the power condition that is 800W in frequency, place 16 hours in room temperature, obtain microwave induced expandable flame retardant silanes crosslinked cable polyolefin jacket material.
Experiment seven:
Microwave induced expandable flame retardant silanes crosslinked cable is as follows by the preparation method of polyolefin jacket material:
One, take low density polyethylene LD100,43g expansion type flame retardant IFR-MT800,3.5g silane coupling A 151, the 2.7g Manganse Dioxide (MnO of 100g drying
2), 1.9g produces aqua zinc borate, 3.2g multi-group crosslink agent TAC, 4.5g crosslinking accelerator tetrachloromethane and 0.37g composite antioxidant, composite antioxidant is comprised of 0.19g antioxidant 300,0.14g oxidation inhibitor tricresyl phosphate benzene methyl and 0.04g DLTP;
Two, each component taken in step 1 is put into to the Banbury mixer banburying of 160 ℃～200 ℃, melting mixing 5min, then by the twin screw extruder granulation of 190 ℃～210 ℃, obtain the sample particle mixed;
Three, the sample particle of mixing is placed in to the vulcanizer compressing tablet, and then be microwave induced crosslinked 60s under 2450MHz, the power condition that is 800W in frequency, place 16 hours in room temperature, obtain microwave induced expandable flame retardant silanes crosslinked cable polyolefin jacket material.
Experiment eight:
Microwave induced expandable flame retardant silanes crosslinked cable is as follows by the preparation method of polyolefin jacket material:
One, low density polyethylene LD615, the 75g expansion type flame retardant IFR-P603,2.2g silane coupling A 171,1.7g carbon black, the 2.5g that take the 100g drying produce aqua AL (OH)
3, 3.4g multi-group crosslink agent TMPAE, 3.5g crosslinking accelerator chlordene methane and 0.4g composite antioxidant, composite antioxidant is comprised of 0.2g oxidation inhibitor 246,0.15g irgasfos 168 and 0.05g DLTP;
Two, each component taken in step 1 is put into to the Banbury mixer banburying of 160 ℃～200 ℃, melting mixing 5min, then by the twin screw extruder granulation of 190 ℃～210 ℃, obtain the sample particle mixed;
Three, the sample particle of mixing is placed in to the vulcanizer compressing tablet, and then be microwave induced crosslinked 60s under 2450MHz, the power condition that is 800W in frequency, place 16 hours in room temperature, obtain microwave induced expandable flame retardant silanes crosslinked cable polyolefin jacket material.
Experiment nine:
Microwave induced expandable flame retardant silanes crosslinked cable is as follows by the preparation method of polyolefin jacket material:
One, ethylene-vinyl acetate copolymer EVA VA18, the 36g expansion type flame retardant IFR-P603,3.5g silane coupling A 171,2.1g barium ferrite, the 2.3g that take the 100g drying produce aqua Mg (OH)
2, 3.2g multi-group crosslink agent TAIC, 3.5g crosslinking accelerator ethylene-tetrafluoroethylene copolymer and 0.35g composite antioxidant, composite antioxidant is comprised of 0.2g antioxidant 1010,0.1g oxidation inhibitor TIOP and 0.05g LSTP;
Two, each component taken in step 1 is put into to the Banbury mixer banburying of 160 ℃～200 ℃, melting mixing 5min, then by the twin screw extruder granulation of 190 ℃～210 ℃, obtain the sample particle mixed;
Three, the sample particle of mixing is placed in to the vulcanizer compressing tablet, and then be microwave induced crosslinked 60s under 2450MHz, the power condition that is 800W in frequency, place 16 hours in room temperature, obtain microwave induced expandable flame retardant silanes crosslinked cable polyolefin jacket material.
Experiment ten:
Microwave induced expandable flame retardant silanes crosslinked cable is as follows by the preparation method of polyolefin jacket material:
One, ethylene-vinyl acetate copolymer EVA VA28, the 43g expansion type flame retardant IFR-P603,3.7g silane coupling A 151,2.5g graphite, the 2.3g that take the 100g drying produce aqua Al (OH)
3, 3.5g multi-group crosslink agent TAIC, 3.1g crosslinking accelerator ethene fluoride copolymers and 0.25g composite antioxidant, composite antioxidant is comprised of 0.15g antioxidant 300,0.06g oxidation inhibitor Tritolyl Phosphate and 0.04g DLTP;
Two, each component taken in step 1 is put into to the Banbury mixer banburying of 160 ℃～200 ℃, melting mixing 5min, then by the twin screw extruder granulation of 190 ℃～210 ℃, obtain the sample particle mixed;
Three, the sample particle of mixing is placed in to the vulcanizer compressing tablet, and then be microwave induced crosslinked 60s under 2450MHz, the power condition that is 800W in frequency, place 16 hours in room temperature, obtain microwave induced expandable flame retardant silanes crosslinked cable polyolefin jacket material.
Test 11:
Microwave induced expandable flame retardant silanes crosslinked cable is as follows by the preparation method of polyolefin jacket material:
One, take the high density polyethylene 5000s of 75g drying and LLDPE7042,43g expansion type flame retardant IFR-T800,2.8g silane coupling A 171, the 2.5g Manganse Dioxide (MnO of 25g drying
2), 1.5g produces aqua Mg (OH)
2, 3.5g multi-group crosslink agent TMPTA, 2.8g crosslinking accelerator ethylene tetrafluoroethylene copolymer and 0.3g composite antioxidant, composite antioxidant is comprised of 0.15g antioxidant 1010,0.07g irgasfos 168 and 0.08g DTDTP;
Two, each component taken in step 1 is put into to the Banbury mixer banburying of 160 ℃～200 ℃, melting mixing 5min, then by the twin screw extruder granulation of 190 ℃～210 ℃, obtain the sample particle mixed;
Three, the sample particle of mixing is placed in to the vulcanizer compressing tablet, and then be microwave induced crosslinked 60s under 2450MHz, the power condition that is 800W in frequency, place 16 hours in room temperature, obtain microwave induced expandable flame retardant silanes crosslinked cable polyolefin jacket material.
Test 12:
By the experiment one～test the 11 microwave induced expandable flame retardant silanes crosslinked cables that make to make the 105mm that thickness is 1.0mm * 145mm sheet material with the polyolefin jacket material, be placed in microwave equipment, the frequency adopted is that the microwave that 2450MHz, power are 800W carries out induced cross-linking, after reaction 60s, in room temperature, place 16 hours.Detect this experiment according to JB/T10436-2004 " electric wire crosslinkable flame retardant polyolefine material " and obtain microwave induced expandable flame retardant silanes crosslinked cable polyolefin jacket material, detected result is as shown in table 1:
Table 1
In JB/T10436-2004 " electric wire crosslinkable flame retardant polyolefine material ", to 125 ℃ of low-smoke non-halogen flame-retardant silane cross-linked polyolefin electric wire and cable jacket materials of heatproof, be: tensile strength >=10.5MPa, elongation at break >=250%, oxygen index >=29.As shown in Table 1, microwave induced expandable flame retardant silanes crosslinked cable meets in JB/T10436-2004 " electric wire crosslinkable flame retardant polyolefine material " 125 ℃ of low-smoke non-halogen flame-retardant silane cross-linked polyolefin electric wire and cable jacket tensile strength of material of heatproof, elongation at break, the desired performance index of oxygen index by the performance index of polyolefin jacket material.
Experiment one～test the 11 microwave induced expandable flame retardant silanes crosslinked cables that prepare to use the polyolefin jacket material all by 158 ℃ * 168h thermal ageing test.
Test 13: the performance of microwave induced crosslinked with silicane and crosslinking electron beam irradiation, peroxide crosslinking, common poach crosslinked with silicane flame-proof polyethylene sheath material is carried out to the contrast experiment:
The polyethylene LLDPE7042 of the experiment one microwave induced crosslinked with silicane made is made to the sheet material that thickness is 1.0mm, through frequency, be that 2450MHz, power are the microwave induced crosslinked of 800W, after reaction times 60s, place 16 hours in room temperature, obtain the sample of microwave induced crosslinked with silicane expandable flame retardant cable with the polyolefin jacket material.
The experiment one microwave induced crosslinked with silicane expandable flame retardant cable obtained is carried out to performance comparison with polyolefin jacket material and the fire-retardant polyethylene material (thickness is 1.0mm) of the crosslinking electron beam irradiation prepared with LLDPE7042, peroxide crosslinking, common poach crosslinked with silicane, and result is as shown in table 2:
Table 2
As shown in Table 2, microwave induced crosslinked with silicane expandable flame retardant cable compares with polyolefin jacket material and the flame-retardant polyolefin sheathed material obtained with other three kinds of crosslinking methods, the gel content of microwave induced crosslinked with silicane expansible flame-proof polythene material is crosslinked apparently higher than alternate manner, and tensile strength, heat extension and oxygen index are apparently higher than the crosslinked with silicane material of poach, and the facility investment of microwave induced crosslinking is low, simple to operate, protection easily, energy-conserving and environment-protective, production efficiency is high, the cost of product is low, the high-temperature stability of products obtained therefrom and good mechanical performance.
Claims (10)
1. microwave induced expandable flame retardant silanes crosslinked cable polyolefin jacket material, it is characterized in that microwave induced expandable flame retardant silanes crosslinked cable with the polyolefin jacket material by weight by the polyolefin resin of 100 parts of dryings, 25～80 parts of expansion type flame retardants, 0.1～4 part of silane coupling agent, 0.2～3 part of microwave absorption, 0.1～4 part produce aqua, 0.3～5 part of multi-group crosslink agent, 0.01～5 part of crosslinking accelerator and 0.07～0.5 part of oxidation inhibitor and make.
2. microwave induced expandable flame retardant silanes crosslinked cable polyolefin jacket material according to claim 1, is characterized in that described polyolefin resin is a kind of in high density polyethylene(HDPE), medium-density polyethylene, Low Density Polyethylene, low density linear polyethylene, ethylene-vinyl acetate copolymer and polyolefin elastomer or wherein several combination.
3. microwave induced expandable flame retardant silanes crosslinked cable polyolefin jacket material according to claim 1, is characterized in that described expansion type flame retardant is a kind of in expansion type flame retardant IFR-P500, expansion type flame retardant IFR-P601, expansion type flame retardant IFR-P602, expansion type flame retardant IFR-P603, expansion type flame retardant IFR-T800 and expansion type flame retardant IFR-MT800 or wherein several combination.
4. microwave induced expandable flame retardant silanes crosslinked cable polyolefin jacket material according to claim 1, is characterized in that described microwave absorption is a kind of in carbon black, graphite, Manganse Dioxide and barium ferrite or wherein several combination.
5. microwave induced expandable flame retardant silanes crosslinked cable polyolefin jacket material according to claim 1, is characterized in that described product aqua is a kind of in magnesium hydroxide, aluminium hydroxide, zinc borate and Cadmium sulfate hydrate or wherein several combination.
6. microwave induced expandable flame retardant silanes crosslinked cable polyolefin jacket material according to claim 1, it is characterized in that described silane coupling agent is vinyltrimethoxy silane, vinyltriethoxysilane, a kind of in γ aminopropyltriethoxy silane, benzene n-formyl sarcolysine ethyl triethoxy silicane alkane, γ-second phenodiazine base propyl trimethoxy silicane, β-(3,4-epoxycyclohexyl) ethyl trimethoxy silane and γ-propyl methacrylate base Trimethoxy silane or wherein several combination.
7. microwave induced expandable flame retardant silanes crosslinked cable polyolefin jacket material according to claim 1, is characterized in that described multi-group crosslink agent is a kind of in triallyl cyanurate, cyamelide triallyl, trimethylolpropane tris (methyl) acrylate, trimethylolpropane tris allyl ether, tetramethylolmethane three allyl ethers, tetramethylolmethane tetraene propyl ether and triglycol methacrylic ester or wherein several combination.
8. microwave induced expandable flame retardant silanes crosslinked cable polyolefin jacket material according to claim 1, it is characterized in that described crosslinking accelerator is ethylene-tetrafluoroethylene copolymer, ethene-1, a kind of in chlorotrifluoroethylcopolymer copolymer, ethene-fluoride copolymers, hexachloroethane and tetrachloromethane or wherein several combination.
9. microwave induced expandable flame retardant silanes crosslinked cable polyolefin jacket material according to claim 1, is characterized in that described oxidation inhibitor is phenolic antioxidant, phosphite ester kind antioxidant, phosphoric acid ester oxidation inhibitor and containing the mixture of two or more composition in the thioesters kind antioxidant;
Described phenolic antioxidant is 2,6-di-tert-butylphenol, 2,4,6-tri-tert-butylphenol, 4,4 '-thiobis (6-tertiary butyl-3-methylphenol) or four [methylene radical-3-(3 ', 5 '-di-tert-butyl-4 '-hydroxy phenyl) propionic acid] pentaerythritol ester;
Described phosphite ester kind antioxidant is triphenyl phosphite, tricresyl phosphite (2,4-di-tert-butyl phenyl) ester or the different monooctyl ester of tricresyl phosphite;
Described phosphoric acid ester oxidation inhibitor is the tricresyl phosphate benzene methyl;
Described is Tyox B, thio-2 acid bay octadecyl ester or thio-2 acid two (13) ester containing the thioesters kind antioxidant.
10. the preparation method of polyolefin jacket material for the described microwave induced expandable flame retardant silanes crosslinked cable of claim 1 is characterized in that microwave induced expandable flame retardant silanes crosslinked cable is as follows by the preparation method of polyolefin jacket material:
One, take by weight 100 parts of polyolefin resines 80 ℃～120 ℃ of dryings, 25～80 parts of expansion type flame retardants, 0.1～4 part of silane coupling agent, 0.2～3 part of microwave absorption, 0.1～4 part of product aqua, 0.3～5 part of multi-group crosslink agent, 0.01～5 part of crosslinking accelerator and 0.07～0.5 part of oxidation inhibitor;
Two, at 160 ℃～200 ℃, polyolefin resin, expansion type flame retardant, silane coupling agent, microwave absorption, product aqua, multi-group crosslink agent, crosslinking accelerator and oxidation inhibitor are carried out to melting mixing 5min, then by the twin screw extruder granulation of 190 ℃～210 ℃, obtain the sample particle mixed;
Three, the sample particle of mixing is placed in to the vulcanizer compressing tablet, and then be microwave induced crosslinked 40s～80s under 2450MHz, the power condition that is 650W～1000W in frequency, place 16 hours in room temperature, obtain microwave induced expandable flame retardant silanes crosslinked cable polyolefin jacket material.
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