CN103333403A - Halogen-free intumescent flame retardant polyolefine cable sheath material and preparation method thereof - Google Patents
Halogen-free intumescent flame retardant polyolefine cable sheath material and preparation method thereof Download PDFInfo
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- CN103333403A CN103333403A CN2013102710053A CN201310271005A CN103333403A CN 103333403 A CN103333403 A CN 103333403A CN 2013102710053 A CN2013102710053 A CN 2013102710053A CN 201310271005 A CN201310271005 A CN 201310271005A CN 103333403 A CN103333403 A CN 103333403A
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Abstract
The invention relates to a composite for a halogen-free intumescent flame retardant polyolefine cable sheath material and a preparation method thereof. The composite is made into a sheath composite by mixing polyethylene resin, ethylene vinyl acetate copolymer resin, an ethylene-vinyl acetate grafted maleic anhydride copolymer, ammonium polyphosphate, pentaerythritol, a halloysite nanotube, an antioxidant, a silane coupling agent and polyethylene wax, wherein the ethylene vinyl acetate copolymer resin contains 18% by weight of VA. Because the composite is added, the halogen-free intumescent flame retardant polyolefine cable sheath material disclosed by the invention has the advantages that the tensile strength is enhanced by about 20%, the breaking elongation enhancement is basically kept unchanged, the limited oxygen index is enhanced to about 29%, the vertical burning grade achieves a V0 grade, the peak heat release rate of a polyolefine cable sheath material during burning is reduced to about 200 kW/m<2> and the total release amount is reduced to about 80 Mj/m<2>.
Description
Technical field
The present invention relates to a kind of halogen-free expanded flame-retardant polyolefin cable sheath material composition and method of making the same, belong to the CABLE MATERIALS technical field.
Technical background
The polyolefins macromolecular material is widely used as insulating material because good filling and physical and mechanical properties has been widely used in the cable and wire industry.But the polyolefins macromolecular material very easily burns, and makes its range of application be subjected to great restriction.Halogen flame flame retarding efficiency height, but consider that European Union and the public are to the pay attention to day by day of environmental protection, the increasing pressure is received in the application of halogen flame in electric wire, study novel halogen-free flame-retardant system, development environment-friendly cable electric wire flame-retarded technology, become fire-retardant the reach of science trend.
The expandable flame retardant system becomes one of a kind of emerging halogen-free flame-retardant system, generally is made up of acid source, carbon source and source of the gas.Ammonium polyphosphate is the most frequently used acid source and source of the gas, and tetramethylolmethane is the most frequently used carbon source; The fire retardant mechanism of IFR is that the acid source that is heated to certain temperature can discharge acid and promotes into charcoal with polyvalent alcohol esterification dehydration, expands under the effect of the rare gas element that discharges of source of the gas very much, forms the charcoal layer with the effect of heat insulation resistance oxygen.Because its addition is bigger, so the mechanical property of material is subjected to greater loss, and during less addition, its flame retardant properties is difficult to again improve.So seek a kind of novel fire-retardant synergistic weighting material that has, improve its flame retarding efficiency, can replenish owing to add the caused mechanical property loss of energy of expanding fire retardant simultaneously, be a very significant job.
Summary of the invention
The composition and method of making the same that the purpose of this invention is to provide a kind of halogen-free expanded flame-retardant polyolefin cable oversheath material, the composition that solves existing halogen-free expanded flame-retardant cable jacket material is cost reaching when improving fire-retardant purpose with other performance of damaging this material because of the expanding fire retardant that adopts, exist the mechanical property of material to be subjected to the deficiency of greater loss, when being implemented in the flame retardant properties of further raising material by the present invention, do not influence the material body performance, the mechanical property of strongthener promotes quality product.
The objective of the invention is to be achieved through the following technical solutions, a kind of composition of halogen-free expanded flame-retardant polyolefin cable oversheath material, the polyvinyl resin that comprises mass percent 10%-20%, the ethylene-vinyl acetate copolymer base-material of 35%-45%, the ethylene-vinyl acetate grafted maleic anhydride multipolymer compatilizer of 5%-10%, the ammonium polyphosphate flame retardant of 18%-24%, the tetramethylolmethane fire retardant of 6%-8%, the processing aid of 1%-2%, the oxidation inhibitor of 1%-2%, the silane coupling agent of 1%-2%, it is characterized in that, described composition also comprises halloysite nanotubes, and its mass percent is 1-3%.
The preparation of compositions method of halogen-free expanded flame-retardant polyolefin cable oversheath material is characterized in that, may further comprise the steps:
1) silane coupling agent that weighs halloysite nanotubes, the 1%-2% of 1-3% adds in the homogenizer and mixes more than 5 minutes;
2) above-mentioned 1) compound in weigh ammonium polyphosphate flame retardant, the 6%-8% of 18%-24% the tetramethylolmethane fire retardant add in the homogenizer and mix more than 5 minutes;
3) above-mentioned 2) compound in add the polyvinyl resin of 10%-20%, the ethylene-vinyl acetate copolymer base-material of 35%-45%, the ethylene-vinyl acetate grafted maleic anhydride multipolymer compatilizer of 5%-10%, the processing aid of 1%-2% successively, the oxidation inhibitor of 1%-2% adds in the homogenizer and mixes more than 3 minutes;
4) with above-mentioned 3) material that mixes joins melt blending in two roller mills, and blending temperature is 140 ℃-160 ℃, and the time is 10-15min.
The present invention introduces halogen-free expanded flame-retardant polyolefin cable sheath material with halloysite nanotubes, and halloysite nanotubes (HNTs) is the cheap natural nano pipe that has than big L/D ratio of a kind of well-crystallized, and strengthening action is preferably arranged.It has compared following advantage with carbon nanotube: low price, wide material sources; Hydroxyl is contained on its surface, is fit to further modification.It is rich in Si-O key and Al-O key simultaneously, and is similar with polynite, can promote to form more stable charcoal layer when polymer combustion.Therefore has potential using value aspect polymkeric substance halogen-free flameproof and the increase thermostability.Traditional expandable flame retardant is cost reaching when improving fire-retardant purpose with other performance of damaging this material, and halloysite nanotubes is because the characteristic of self structure and composition, reaching the flame-retardant modified purpose while, do not influence the material body performance, strengthened the mechanical property of material simultaneously, and technology is simple, is convenient to operation control, material cost is low, wide material sources.Adopt halogen-free expanded flame-retardant polyolefin cable sheath material of the present invention with the halogen-free expanded flame-retardant polyolefin cable oversheath material of preparation of compositions good mechanical performance and flame retardant properties to be arranged.
Specific implementation method
Further specify the present invention in conjunction with the embodiments, the present invention includes the polyvinyl resin of the 10%-20% of mass percent, the ethylene-vinyl acetate copolymer base-material of 35%-55%, the ethylene-vinyl acetate grafted maleic anhydride multipolymer compatilizer of 5%-10%, the ammonium polyphosphate flame retardant of 18%-24%, the tetramethylolmethane fire retardant of 6%-8%, the processing aid of 1%-2%, the oxidation inhibitor of 1%-2%, the silane coupling agent of 1%-2% and mass percent are the halloysite nanotubes of 1%-3%.
Embodiment one: weigh 2% halloysite, 1.5% silane coupling agent, pour in the homogenizer and mix more than 5 minutes; Weigh 21% ammonium polyphosphate flame retardant again, 7% tetramethylolmethane fire retardant is poured in the homogenizer and is mixed more than 5 minutes; Adding 55% vinyl acetate content then successively and be 18% ethylene vinyl acetate resin, 15% polyethylene, ethene-vinyl acetate-copolymer-maleic anhydride compatilizer of 4%, 2% oxidation inhibitor, 1% releasing agent mixes more than 3 minutes; Oxidation inhibitor is four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester, and processing aid is polyethylene wax, and silane coupling agent is γ-An Bingjisanyiyangjiguiwan.The material that mixes is joined in two roller mills, carry out melt blending, make the composition that halogen-free expanded flame-retardant polyolefin cable oversheath material of the present invention is used.
Resulting composition is vulcanized in vulcanizer in flakes, and curing temperature is 160 ℃, and the time is 8min, makes limiting oxygen index(LOI), vertical combustion test bars and Mechanics Performance Testing batten and taper calorimetric test sample then.Its test result is as shown in table 1.
Embodiment two, weigh 1.5% halloysite, 1% silane coupling agent, pour in the homogenizer and mix more than 5 minutes; Weigh 21% ammonium polyphosphate flame retardant again, 7% tetramethylolmethane fire retardant is poured in the homogenizer and is mixed more than 5 minutes; Adding 55% vinyl acetate content then successively and be 18% ethylene vinyl acetate resin, 15% polyvinyl resin, ethene-vinyl acetate-copolymer-maleic anhydride compatilizer of 6%, 2% oxidation inhibitor, 1% releasing agent mixes more than 3 minutes; Oxidation inhibitor is four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester, and processing aid is polyethylene wax, and silane coupling agent is γ-An Bingjisanyiyangjiguiwan.The material that mixes is joined in two roller mills, carry out melt blending, make the composition that halogen-free expanded flame-retardant polyolefin cable oversheath material of the present invention is used.
Resulting composition is vulcanized in vulcanizer in flakes, and curing temperature is 160 ℃, and the time is 8min, makes limiting oxygen index(LOI), vertical combustion test bars and Mechanics Performance Testing batten and taper calorimetric sample then.Its test result is as shown in table 1.
Embodiment two, weigh 3% halloysite, 2% silane coupling agent, pour in the homogenizer and mix more than 5 minutes; Weigh 21% ammonium polyphosphate flame retardant again, 7% tetramethylolmethane fire retardant is poured in the homogenizer and is mixed more than 5 minutes; Adding 55% vinyl acetate content then successively and be 18% ethylene vinyl acetate resin, 15% polyvinyl resin, ethene-vinyl acetate-copolymer-maleic anhydride compatilizer of 6%, 2% oxidation inhibitor, 1% releasing agent mixes more than 3 minutes; Oxidation inhibitor is four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester, and processing aid is polyethylene wax, and silane coupling agent is γ-An Bingjisanyiyangjiguiwan.The material that mixes is joined in two roller mills, carry out melt blending, make the composition that halogen-free expanded flame-retardant polyolefin cable oversheath material of the present invention is used.
Resulting composition is vulcanized in vulcanizer in flakes, and curing temperature is 160 ℃, and the time is 8min, makes limiting oxygen index(LOI), vertical combustion test bars and Mechanics Performance Testing batten and taper calorimetric sample then.Its test result is as shown in table 1.
Comparative Examples one weighs 21% ammonium polyphosphate flame retardant, and 7% tetramethylolmethane fire retardant is poured in the homogenizer and mixed more than 5 minutes; Adding 64% vinyl acetate content then successively and be 18% ethylene vinyl acetate resin, ethene-vinyl acetate-copolymer-maleic anhydride compatilizer of 6%, 2% oxidation inhibitor, 1% processing aid mixes more than 3 minutes; Oxidation inhibitor is four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester, and processing aid is polyethylene wax.The material that mixes is joined in two roller mills, carry out melt blending, make the composition that halogen-free expanded flame-retardant polyolefin cable oversheath material of the present invention is used.
Resulting composition is vulcanized in vulcanizer in flakes, and curing temperature is 160 ℃, and the time is 8min, makes limiting oxygen index(LOI) and vertical combustion test bars and Mechanics Performance Testing batten then.Its test result is as shown in table 1.
Table 1
| Embodiment/Comparative Examples | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative Examples 1 |
| Tensile strength (MPa) | 13 | 14 | 13 | 10 |
| Elongation at break (%) | 310 | 290 | 320 | 310 |
| Limiting oxygen index(LOI) (%) | 29 | 29.5 | 29 | 28 |
| Vertical combustion test (UL-94) | V0 | V0 | V0 | V0 |
| Heat release rate (kW/m 2） | 223 | 198 | 210 | 275 |
| Total heat burst size (MJ/m 2） | 83 | 81 | 79 | 116.8 |
| Heat discharges time to peak (s) | 312 | 285 | 301 | 155 |
By table 1 data as can be known, the tensile strength of the material ratio that compares improves 30%-40% among the embodiment, and elongation at break slightly improves, and the intensity of material improves the application that can guarantee some occasion material.It is about 1% that limiting oxygen index(LOI) improves, and the heat release rate of material reduces obviously, and the total heat burst size reduces about 18%-28%, and the time lengthening that reaches maximum heat rate of release peak value after the burning is about original 2 times.As seen, at very little addition, during less cost, the thermal characteristics of material and flame retardant properties have significantly and promote, and have reduced the danger that fire takes place.Even presence of fire, the reduction of heat release rate and the reduction of hot burst size will reduce the injury that fire causes, and the prolongation that heat discharges time to peak will provide valuable time for rescue and the saving oneself of people of fire.
Claims (2)
1. the composition of a halogen-free expanded flame-retardant polyolefin cable oversheath material, comprise the polyvinyl resin of mass percent 10%-20%, the ethylene-vinyl acetate copolymer base-material of 35%-45%, the ethylene-vinyl acetate grafted maleic anhydride multipolymer compatilizer of 5%-10%, the ammonium polyphosphate flame retardant of 18%-24%, the tetramethylolmethane fire retardant of 6%-8%, the processing aid of 1%-2%, the oxidation inhibitor of 1%-2%, the silane coupling agent of 1%-2%, it is characterized in that, described composition also comprises halloysite nanotubes, and its mass percent is 1-3%.
2. the preparation of compositions method of halogen-free expanded flame-retardant polyolefin cable oversheath material is characterized in that, may further comprise the steps:
1) silane coupling agent that weighs halloysite nanotubes, the 1%-2% of 1-3% adds in the homogenizer and mixes more than 5 minutes;
2) above-mentioned 1) compound in weigh ammonium polyphosphate flame retardant, the 6%-8% of 18%-24% the tetramethylolmethane fire retardant add in the homogenizer and mix more than 5 minutes;
3) above-mentioned 2) compound in add the polyvinyl resin of 10%-20%, the ethylene-vinyl acetate copolymer base-material of 35%-45%, the ethylene-vinyl acetate grafted maleic anhydride multipolymer compatilizer of 5%-10%, the processing aid of 1%-2% successively, the oxidation inhibitor of 1%-2% adds in the homogenizer and mixes more than 3 minutes;
4) with above-mentioned 3) material that mixes joins melt blending in two roller mills, and blending temperature is 140 ℃-160 ℃, and the time is 10min-15min.
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Cited By (7)
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| CN111117054A (en) * | 2019-12-31 | 2020-05-08 | 安徽蒙特尔电缆集团有限公司 | Low-smoke halogen-free flame-retardant B1-grade polyolefin cable sheath material and preparation method thereof |
| CN112037972A (en) * | 2020-08-04 | 2020-12-04 | 远东电缆有限公司 | A-level flexible fireproof cable with combustion performance and preparation process thereof |
| CN113717488A (en) * | 2021-09-06 | 2021-11-30 | 桃江县大丰木业有限责任公司 | Smoke-inhibiting flame-retardant wood composite material and preparation method thereof |
| CN115181352A (en) * | 2022-08-15 | 2022-10-14 | 华北电力大学（保定） | Flame-retardant material for cable sheath and preparation method thereof |
| CN115433439A (en) * | 2022-08-19 | 2022-12-06 | 湖北合聚新材料有限公司 | PET flame-retardant reinforced material and preparation method and application thereof |
| CN116253947A (en) * | 2023-02-01 | 2023-06-13 | 江苏馨德高分子材料股份有限公司 | Halogen-free low-smoke flame-retardant polyolefin sheath material and preparation process thereof |
| EP4185558A4 (en) * | 2020-07-24 | 2024-09-04 | Corning Res & Dev Corp | Flexible indoor/outdoor high-fiber-count cable |
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| CN113717488B (en) * | 2021-09-06 | 2024-07-05 | 桃江县大丰木业有限责任公司 | Smoke-suppression flame-retardant wood composite material and preparation method thereof |
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| CN115433439A (en) * | 2022-08-19 | 2022-12-06 | 湖北合聚新材料有限公司 | PET flame-retardant reinforced material and preparation method and application thereof |
| CN115433439B (en) * | 2022-08-19 | 2023-10-27 | 湖北合聚高分子材料有限公司 | PET flame-retardant reinforcing material, and preparation method and application thereof |
| CN116253947A (en) * | 2023-02-01 | 2023-06-13 | 江苏馨德高分子材料股份有限公司 | Halogen-free low-smoke flame-retardant polyolefin sheath material and preparation process thereof |
| CN116253947B (en) * | 2023-02-01 | 2023-10-27 | 江苏馨德高分子材料股份有限公司 | Halogen-free low-smoke flame-retardant polyolefin sheath material and preparation process thereof |
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Application publication date: 20131002 |