CN1133692C - Prepn of fireproofing cable material without halide - Google Patents
Prepn of fireproofing cable material without halide Download PDFInfo
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- CN1133692C CN1133692C CNB001221574A CN00122157A CN1133692C CN 1133692 C CN1133692 C CN 1133692C CN B001221574 A CNB001221574 A CN B001221574A CN 00122157 A CN00122157 A CN 00122157A CN 1133692 C CN1133692 C CN 1133692C
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Abstract
The present invention relates to a preparation method for a halogen-free flame retarding cable material. The present invention is characterized in that a halogen-free flame retarding cable material is formed in a mode that 67 to 75 wt% of polyolefin is used as a base material, a halogen-free flame retarding agent and small amount of processing aids are added in the polyolefin, and the mixture is extruded by an extruding machine to be cut into granules; the tensile strength is greater than 1.2MPa, the elongation at break is greater than 400%, the oxygen index is 29.6, vertical combustion tests pass the UL-94V-0 grade, and the maximum heat release rate is decreased to 185KW /M<2>; simultaneously, the smoke density and the generating capacity of carbonic oxide are basically the same as that of pure base materials. The halogen-free flame retarding cable material has the advantages of good flow performance, low melt viscosity and good appearance of products.
Description
The present invention relates to flame-retardant electric wire and cable material and preparation method thereof technical field.
The plastics output that the whole world is used for electric wire grows at top speed in recent years, and meanwhile the fire failure that is caused by the plastics burning also becomes an important social issue day by day.But can discharge gases such as a large amount of smog and poisonous, corrosive hydrogen halides during the burning of halogen-containing fire retardant material, hinder people from fire, to withdraw and fire-fighting work, so the exploitation of low-smoke non-halogen flame-retardant technology become a hot issue in the world.
Japanese Patent JP88225640 has described with preparation flame-proof polyethylenes such as polyethylene (PE), magnesium hydroxide, phosphorus flame retardants, and its goods oxygen index (OI) reaches 28.9; European patent EP 280761 has been described with preparation fire-retardant polyethylene cable materials such as ethylene-vinyl acetate copolymer (EVA), organosilane graft modification EVA, magnesium hydroxides, and goods OI is greater than 35.0; Japanese Patent JP97171721 has described with ethene--90 parts of butylene copolymers, and 10 parts of linear low density polyethylenes (LLDPE) add 120 parts of magnesium hydroxides, 0.5 part of stearic acid, 0.4 part of peroxide initiator, the goods OI after lightly crosslinked is 28.5; Japanese Patent JP93301996 has described with new LDPE (film grade) (LDPE), high density polyethylene(HDPE) (HDPE) and magnesium hydroxide, and fire-retardant product OI reaches 31.2, elongation at break 150%.But aforesaid method is because fire retardants such as employing magnesium hydroxide will reach fire-retardant UL94 V-0 level, and the loading level of required fire retardant big (more than 50%), bad dispersibility cause the mechanical property of goods to descend significantly; And during extrusion moulding, melt viscosity is big, is difficult to processing.
EP0735119A1 (1996) has described a kind of phosphorus-nitrogen expansion type fire retardant; U.S. Hao Si Te-Sai Laimei (Hoechest Celamese) company produces is used for polyethylene and the polypropylene expansion type flame retardant is 35% in the add-on of polyethylene, and oxygen index reaches 35, and UL-94 reaches the V-0 level.But it is undesirable that this expansion type fire retardant is used in the polyethylene flame retardant effect on the one hand, on the other hand the own moisture-sensitive of this based flame retardant and can cause the electric property of its fire-retardant product to descend; Simultaneously, because goods reach the total amount of filling of the required fire retardant of V-0 level about 35%, it is higher that fire-retardant product adds the man-hour melt viscosity, and mechanical property is also undesirable; Also have high this factor of cost also to limit its application in addition.
The international fire retardant in the 3rd Beijing and fire retardant material scientific seminar paper (Proc.IFR ' 99 Beijing, China; P239) reported that acting synergistically on ethylene-propylene rubber(EPR) with expansible black lead and halogen flame decabromodiphynly oxide prepares wire cable material; It is that the feedstock production polyolefin foam is used for automobile and electric equipment products that Japanese Patent 0977894 (1997) and 08295753 (1996) has been described with expansible black lead etc.But it is, poor with this fire retardant polyolefin goods mechanical property and electric property for preparing because the expansible black lead particle diameter is big; The do not require emphasis mechanical property index such as elongation at break particularly of fire retardant polyolefin of foam materials is so can be feedstock production fire retardant polyolefin foam materials with expansible black lead etc. still; But the preparation of CABLE MATERIALS is much more complicated to the requirement of indexs such as mechanical property, electric property, processing characteristics.The Searches of Patent Literature shows, do not see with expansible black lead up to now as yet and has synergistic additive to prepare the report of non-halogen flame-retardant cable.
The present invention propose a kind of with polyolefine as base-material, adopt expansible black lead and the method for synergistic additive preparation fireproofing cable material without halide arranged.
The preparation method of this non-halogen flame-retardant cable is characterized in that: with the polyolefine that accounts for fire-resistant cable material gross weight 67～73% is base-material, adds the halogen-free flame retardants that accounts for fire-resistant cable material gross weight 27～33%; After mixing, again through forcing machine extrude, pelletizing;
In the described polyolefin base material, ethylene-vinyl acetate copolymer (EVA) accounts for 72～100% of base-material gross weight, and linear low density polyethylene (LLDPE) accounts for 0～14% of base-material gross weight, and high density polyethylene(HDPE) (HDPE) accounts for 0～14% of base-material gross weight;
Described halogen-free flame retardants comprises expansible black lead and plays synergistic additive with it;
The expansion multiple of described expansible black lead 25～60, pH value is 7 ± 0.2, particle diameter 80～120 orders, add-on accounts for 7～10% of fire-resistant cable material gross weight;
Described additive comprises one or more combinations in zinc borate or the P-N type fire retardant;
Described P-N type fire retardant comprises red phosphorus, ammonium polyphosphate (APP), trimeric cyanamide or the organophosphorus nitrogen expansion type fire retardant tetramethylolmethane phosphoric acid fat trimeric cyanamide salt compounds (NP28) of particle diameter 5～30 μ m that adopt melamino-formaldehyde resin capsule material micro encapsulation; Wherein the add-on of micro encapsulation red phosphorus is 0～5% of a fire-resistant cable material gross weight, and other P-N type fire retardant is added up and accounted for 0～20% of fire-resistant cable material gross weight;
Described zinc borate add-on is 0～23% of a fire-resistant cable material gross weight.
Add the performance of an amount of processing aid can improve the material extrusion moulding time, described processing aid can be selected from the organic fluorine compounds dynamar that Minnesota Mining and Manufacturing Company produces, and add-on is 0.1～0.2% of a fire-resistant cable material gross weight.
The thermal weight loss test shows, the fireproofing cable material without halide product of the present invention after adding expansible black lead and synergistic additive being arranged, and its oxidate temperature has improved 50-70 ℃.
The non-halogen flame-retardant cable elongation at break of prior art for preparing is not more than 200% usually, and tensile strength is not more than 1.1MPa, the melt viscosity height; And the non-halogen flame-retardant cable tensile strength of the present invention preparation is greater than 1.2MPa, and elongation at break is greater than 400%, and oxygen index is 29.6, and testing vertical flammability is by UL-94 V-0 level.
The combustion test of tapered calorimeter shows that (radiation flux is 35kW/M
2), the non-halogen flame-retardant cable for preparing in the embodiment of the invention is compared with not fire-retardant EVA (VA=19%) CABLE MATERIALS, and the maximum heat rate of release is from 1195kW/M
2Drop to 200kW/M
2About, and smoke density is littler than pure EVA, the carbon monoxide generating capacity is constant substantially.
The present invention since selected particle diameter less than 100 purpose expansible black leads and with its consistency base-material good and that have better mechanical property, selected the halogen-free flame retardants that has fine synergistic effect with expansible black lead simultaneously for use, goods reach the total amount of filling of the required fire retardant of V-0 level little (between 25%～30%), so fire-resistant cable material has mechanical property, electric property preferably; Because expansible black lead and polyolefinic consistency are good, so the melt viscosity of goods is low and have a better machining property; The adding processing aid can reduce the long-pending grain phenomenon of extrusion, guarantees evenly extruding of melt.Non-halogen flame-retardant cable rheological property with the present invention's preparation is better, and melt viscosity is low, and goods have outward appearance preferably.Fire retardant polyolefin of the present invention has reached the index request of non-halogen flame-retardant cable, can be used as fire-resistant cable material and uses.
Non-halogen flame-retardant cable product of the present invention, its fire retardant mechanism is to produce a kind of extremely low fine and close carbon-coating of thermal conductivity of high level expansion between flame and material, this carbon-coating can reduce the heating temperature of material greatly, while, the degree of oxidation of material reduced greatly owing to the effect of the obstruct oxygen of fire-retardant carbon-coating; Phosphorus nitrogen element in the organophosphorus nitrogen expansion type flame retardant molecule can dilute and stop the reaction of living radical in gas phase, thereby reaches fire-retardant purpose; In addition, adding zinc borate has fire-retardant and but cigarette double effects.
Below be embodiments of the invention.
Embodiment 1:
Get 70 parts of the EVA CABLE MATERIALS of VA=19% by weight, expansion multiple is 10 parts of 25 expansible black leads, 20 parts of the organophosphorus nitrogen expansion type fire-retardant N P28 that Fine Chemical Works produces are only demonstrate,proved in Shenzhen, the organic fluorine compounds dynamar that processing aid selects for use Minnesota Mining and Manufacturing Company to produce, add-on is 0.1% of a fire-resistant cable material gross weight, with above-mentioned raw materials after high-speed mixer just mixes, again through twin screw extruder extrude, pelletizing.Three sections processing temperatures of twin screw extruder are 150～160 ℃, 180～200 ℃ and 165～175 ℃.The combustion test of tapered calorimeter shows that (radiation flux is 35kW/M
2), the non-halogen flame-retardant cable of present embodiment preparation is compared with not fire-retardant EVA (VA=19%) CABLE MATERIALS, and the maximum heat rate of release is from 938kW/M
2Drop to 200kW/M
2About, and smoke density is littler than pure EVA, the carbon monoxide generating capacity is constant substantially; Tensile strength is 1.25MPa, and elongation at break is greater than 560%, and oxygen index is 29.2, and combustion test is by UL-94 V-0 level.
Embodiment 2:
Get 67 parts of EVA (VA=19%) CABLE MATERIALS by weight, expansion multiple is 10 parts of 60 expansible black leads, 23 parts of zinc borates, the organic fluorine compounds dynamar that processing aid selects for use Minnesota Mining and Manufacturing Company to produce, add-on is 0.1% of a fire-resistant cable material gross weight,, with above-mentioned raw materials after high-speed mixer just mixes, again through twin screw extruder extrude, pelletizing.Three sections processing temperatures of twin screw extruder are 150～160 ℃, 180～200 ℃ and 175～185 ℃.
The combustion test of tapered calorimeter shows that (radiation flux is 35kW/M
2), the non-halogen flame-retardant cable of present embodiment preparation is compared with not fire-retardant EVA (VA=19%) CABLE MATERIALS, and the maximum heat rate of release is from 1195kW/M
2Drop to 185kW/M
2, smoke density and carbon monoxide generating capacity are all little than pure EVA (VA=19%) CABLE MATERIALS simultaneously; Tensile strength is 1.10MPa, and elongation at break is greater than 380%, and oxygen index is 29.5, and testing vertical flammability is by UL-94 V-0 level.
Embodiment 3:
Get 73 parts of EVA (VA=19%) CABLE MATERIALS by weight, expansion multiple is 7 parts of 60 expansible black leads, APP5 part, micro encapsulation red phosphorus is 4 parts, 11 parts of trimeric cyanamides, processing aid organic fluorine compounds dynamar add-on is 0.1% of a fire-resistant cable material gross weight, with above-mentioned raw materials after high-speed mixer just mixes, again through twin screw extruder extrude, pelletizing.Three sections processing temperatures of twin screw extruder are 145～160 ℃, 170～180 ℃ and 165～180 ℃.
Testing vertical flammability shows that the non-halogen flame-retardant cable of present embodiment preparation puts out certainly from fire; The amount of being fuming is littler than pure EVA (VA=19%) CABLE MATERIALS, and oxygen index is 30.3, and testing vertical flammability is by UL-94 V-0 level.
Embodiment 4:
Get 70 parts of EVA (VA=19%) CABLE MATERIALS by weight, expansion multiple is 10 parts of 25 expansible black leads, NP2815 part, micro encapsulation red phosphorus is 5 parts, with above-mentioned raw materials after high-speed mixer just mixes, again through twin screw extruder extrude, pelletizing.Three sections processing temperatures of twin screw extruder are 145～160 ℃, 170～180 ℃ and 165～180 ℃.
The combustion test of tapered calorimeter shows that (radiation flux is 35kW/M
2), the non-halogen flame-retardant cable of present embodiment preparation is compared with not fire-retardant EVA (VA=19%) CABLE MATERIALS, and the maximum heat rate of release is from 1195kW/M
2Drop to 190kW/M
2, active combustion heat also is reduced to 35MJ/kg; Tensile strength is 1.090MPa, and elongation at break is greater than 450%, and oxygen index is 29.6, and testing vertical flammability is by UL-94 V-0 level.
Embodiment 5:
Get 52 parts of EVA (VA=19%) CABLE MATERIALS by weight, LLDPE10 part, HDPE10 part, expansion multiple is 10 parts of 60 expansible black leads, NP28 is 15 parts, 3 parts in micro encapsulation red phosphorus, and processing aid dynamar add-on is for being 0.2% of fire-resistant cable material gross weight, with above-mentioned raw materials after high-speed mixer just mixes, again through twin screw extruder extrude, pelletizing.Three sections processing temperatures of twin screw extruder are 145～160 ℃, 170～190 ℃ and 175～185 ℃.
The combustion test of tapered calorimeter shows that (radiation flux is 35kw/m
2), the non-halogen flame-retardant cable of present embodiment preparation is compared with not fire-retardant LLDPE, and the maximum heat rate of release has reduced by 5 times, active combustion heat also reduces greatly, oxygen index is greater than 29.4, and testing vertical flammability has outward appearance and melt extrusion properties preferably simultaneously by UL-94 V-0 level.
Embodiment 6:
Get 68 parts of EVA (VA=19%) CABLE MATERIALS by weight, get 5 parts of LLDPE CABLE MATERIALS, expansion multiple is 7 parts of 60 expansible black leads, APP5 part, micro encapsulation red phosphorus is 3 parts, 12 parts of trimeric cyanamides, and processing aid dynamar add-on is for being 0.2% of fire-resistant cable material gross weight, with above-mentioned raw materials after high-speed mixer just mixes, again through twin screw extruder extrude, pelletizing.Three sections processing temperatures of twin screw extruder are 145～160 ℃, 175～180 ℃ and 180～185 ℃.
Testing vertical flammability shows that from putting out, the amount of being fuming is little from fire for the non-halogen flame-retardant cable of present embodiment preparation, and mechanical property is better, and oxygen index is 31.2, and combustion test is by UL-94 V-0 level.Rheological test shows that melt viscosity is little when melt extruding, surperficial zero defect, no melt fracture phenomenon.
Claims (4)
1, a kind of preparation method of non-halogen flame-retardant cable is characterized in that: with the polyolefine that accounts for fire-resistant cable material gross weight 67～73% is base-material, adds the halogen-free flame retardants that accounts for fire-resistant cable material gross weight 27～33%; After mixing, again through forcing machine extrude, pelletizing;
In the described polyolefin base material, ethylene-vinyl acetate copolymer (EVA) accounts for 72～100% of base-material gross weight, and linear low density polyethylene (LLDPE) accounts for 0～14% of base-material gross weight, and high density polyethylene(HDPE) (HDPE) accounts for 0～14% of base-material gross weight.
Described halogen-free flame retardants comprises expansible black lead and plays synergistic additive with it;
The expansion multiple of described expansible black lead 25～60, pH value is 7 ± 0.2, particle diameter 80～120 orders, it is 7～10% that add-on accounts for the fire-resistant cable material gross weight;
Described additive comprises one or more combinations in zinc borate or the P-N type fire retardant.
2, the preparation method of non-halogen flame-retardant cable according to claim 1 is characterized in that: described P-N type fire retardant comprises red phosphorus, ammonium polyphosphate (APP), trimeric cyanamide or the organophosphorus nitrogen expansion type fire retardant tetramethylolmethane phosphoric acid fat trimeric cyanamide salt compounds (NP28) of the particle diameter 5～30um that adopts melamino-formaldehyde resin capsule material micro encapsulation; Wherein the add-on of micro encapsulation red phosphorus is 0～5% of a fire-resistant cable material gross weight, and other P-N type fire retardant is added up and accounted for the 0-20% of fire-resistant cable material gross weight.
3, the preparation method of non-halogen flame-retardant cable according to claim 1 is characterized in that described zinc borate accounts for the 0-23% of fire-resistant cable material gross weight.
4, the preparation method of non-halogen flame-retardant cable described in claim 1, it is characterized in that to add an amount of processing aid, described processing aid can be selected from the organic fluorine compounds dynamar that Minnesota Mining and Manufacturing Company produces, and add-on is 0.1～0.2% of a fire-resistant cable material gross weight.
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| CNB001221574A CN1133692C (en) | 2000-07-22 | 2000-07-22 | Prepn of fireproofing cable material without halide |
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|---|---|---|---|
| CNB001221574A CN1133692C (en) | 2000-07-22 | 2000-07-22 | Prepn of fireproofing cable material without halide |
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| CN1335334A CN1335334A (en) | 2002-02-13 |
| CN1133692C true CN1133692C (en) | 2004-01-07 |
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