CN101560314A - Halogen-free phosphorus-free inflaming retarding polyolefine material prepared by radiation grafting technology, preparation method and the application thereof - Google Patents
Halogen-free phosphorus-free inflaming retarding polyolefine material prepared by radiation grafting technology, preparation method and the application thereof Download PDFInfo
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Abstract
The invention provides a halogen-free phosphorus-free inflaming retarding polyolefine material prepared by radiation grafting technology, a preparation method and application thereof. The material takes ethylene-vinylacetate copolymer with maleic anhydride functional group (EVA-g-MAH) prepared by radiation grafting technology as a compatilizer, and a mixture of two or more than two of ethylene-vinylacetate (EVA), ethylene propylene terpolymer rubber (EPDM) and linear low density polyethylene (LLDPE) as a base material. The base material is mixed with a composite antioxidizer, a halogen-free phosphorus-free inflaming retardant (melamine cyanurate (MCA), the composite of Al(OH)3 and Mg(OH)2, and zinc borate), a lubricating agent, a cross-linking additive, and halogen-free masterbatch for twice by a twin screw, and then extruding and granulating are conducted to prepare the polyolefine material. After radiation cross-linking, the safety performance of the wires, cables and heat shrinkable tubing prepared by the material can pass the VW-1 vertical combustion test in standards of UL3266, UL224, and the like .
Description
Technical field
The present invention relates to a kind of halogen-free phosphorus-free inflaming retarding polyolefine material that adopts the radiation grafting technology preparation, can be by the electric wire and the safety performance of thermal contraction casing tube behind radiation crosslinking of this material preparation by VW-1 vertical combustion detection in the standards such as UL3266 and UL224.
" the electronic waste facture " based on two instructions that European Union in 2002 has worked out, one of them instruction for " about in electronic and electrical equipment, banning use of some objectionable impurities instruction " (ROHS).The ROHS requirement, electrical equipment, electronic product that on July 1st, 2006 was thrown in European Union market later on must not contain 6 kinds of objectionable impuritiess such as lead, mercury, cadmium, sexavalent chrome, Polybrominated biphenyl and Poly Brominated Diphenyl Ethers.2004 beginning of the years, the Ministry of Information industry is according to relevant rules such as " promotion law on cleaner production ", " prevention and control of environmental pollution by solid wastes methods ", work out " electronics and IT products prevention and cure of pollution management method " (being called for short " way "), " way " regulation: must not contain 6 kinds of objectionable impuritiess such as lead, mercury, cadmium, sexavalent chrome, Polybrominated biphenyl and Poly Brominated Diphenyl Ethers in electronics, the electric equipment products after 1 day July in 2006, stipulate that simultaneously the electronics, the electric equipment products that enter China must not contain above 6 kinds of objectionable impuritiess.Therefore the low-smoke halide-free fireproof composite polyolefine material that development, exploitation do not contain 6 kinds of objectionable impuritiess stipulating in the instruction becomes at present the focus of developing material both at home and abroad.
It is base material as compatilizer and polyolefine material blend that one of inventor's original unit---Shanghai Applied Physics institute of the Chinese Academy of Sciences adopts the ethylene-vinyl acetate copolymer (EVA-g-MAH) of radiation grafting maleic anhydride in the patent CN200610028750.5 (low-smoke halide-free fireproof composite polyolefine material and its production and application) of application in 2006, phosphorus, nitrogen combustion inhibitor are main flame retardant, prepare 125 ℃ of halogen-free flame retardant heat shrinkable sheathings of heatproof by radiation crosslinking.This patent of invention adopts the synergy of phosphor nitrogen combustion inhibitor, prepare the halogen-free flameproof heat-shrinkable tube that flame retardant properties can detect by VW-1 vertical combustion among the UL224, but forbid clearly that in the existing relevant law of developed countries such as European Union and Japan phosphoric uses in the halogen-free flame-retardant cable material.The present invention has improved former invention, adopts the synergy and the inorganic combustion inhibitor AL (OH) thereof of nitrogen flame retardant and inorganic combustion inhibitor zinc borate
3With Mg (OH)
2The effect of mixture assisting flame-resistant, the ethylene-vinyl acetate copolymer (EVA-g-MAH) that utilizes the radiation grafting maleic anhydride is as the high-performance compatilizer, and can prepare flame retardant properties equally can be by the halogen-free anti-flaming polyolefin material of VW-1 vertical combustion detection among the UL224.
Summary of the invention
The purpose of this invention is to provide a kind of halogen-free phosphorus-free inflaming retarding polyolefine material that adopts the radiation grafting technology preparation, can be by the electric wire and the safety performance of thermal contraction casing tube behind radiation crosslinking of this material preparation by VW-1 vertical combustion detection in the standards such as UL3266 and UL224.
The halogen-free phosphorus-free inflaming retarding polyolefine material of the present invention-employing radiation grafting technology preparation is made up of following substances in parts by weight:
5～15 parts of the ethylene-vinyl acetate copolymers of radiation grafting maleic anhydride (EVA-g-MAH), 65～80 parts of ethylene-vinyl acetate copolymers (EVA), 15～20 parts of linear low density of polyethylene (LLDPE), 0.5～4 part of composite antioxidant, 50～100 parts of melamine cyanurates (MCA), AL (OH)
3With Mg (OH)
210～20 parts of 40～80 parts of mixtures, zinc borates, 1～3 part of divalence metallic soap of stearic acid salt lubricant, 1～3 part of polyethylene wax lubricant, crosslinking coagent be polyfunctional monomer (methyl) acrylate or 0～3 part of triallyl isocyanurate (TAIC), 0～5 part of Halogen Masterbatch, above-mentioned substance is all commercially available.
The halogen-free phosphorus-free inflaming retarding polyolefine material of the present invention-employing radiation grafting technology preparation is made up of following substances in parts by weight:
5～15 parts of the ethylene-vinyl acetate copolymers of radiation grafting maleic anhydride (EVA-g-MAH), 60～70 parts of ethylene-vinyl acetate copolymers (EVA), 5～15 parts of terpolymer EP rubbers (EPDM), 10～20 parts of linear low density of polyethylene (LLDPE), 0.5～4 part of composite antioxidant, 50～100 parts of melamine cyanurates (MCA), AL (OH)
3With Mg (OH)
210～20 parts of 40～80 parts of mixtures, zinc borates, 1～3 part of divalence metallic soap of stearic acid salt lubricant, 1～3 part of polyethylene wax lubricant, crosslinking coagent be polyfunctional monomer (methyl) acrylate or 0～3 part of triallyl isocyanurate (TAIC), 0～5 part of Halogen Masterbatch, above-mentioned substance is all commercially available.
The ethylene-vinyl acetate copolymer of described radiation grafting maleic anhydride (EVA-g-MAH) is by being dissolved in 1～5 part maleic anhydride (MAH) and 100 parts of ethylene-vinyl acetate copolymers (EVA) in 2～10 parts of acetone after high-speed mixer mixes, Deng the granulation in twin screw extruder of acetone volatilization back, again through the rumbatron electron rays or
60Radiation 5～30KGy dosage in the gamma-rays of Co source gets percentage of grafting at 0.5～2% radiation grafting material.
The melting index M of described ethylene-vinyl acetate copolymer (EVA), in 2～6g/min scope, wherein vinyl acetate content is in 14～40% scopes.
Described composite antioxidant is made up of the oxidation inhibitor of following weight ratio: Hinered phenols antioxidant: thioesters kind antioxidant=0.5: 1～3.
Described Hinered phenols antioxidant means: 1,3, and 5-trimethylammonium-2,4,6-three (3,5-di-tert-butyl-4-hydroxybenzyl) benzene, 1,1,3-three (2-methyl-4-hydroxyl-5-t-butyl-phenyl) butane, pentaerythritol ester, β-(3,5-di-tert-butyl-4-hydroxy phenyl) propionic acid octadecyl ester.
The thioesters kind antioxidant means: Tyox B (anti-oxidant DLTP), thio-2 acid (octadecyl ester), thio-2 acid two (14 ester).
The acrylate cross linked auxiliary agent of described polyfunctional monomer (methyl) means: Viscoat 295, three-TRIM, pentaerythritol triacrylate.
Described Halogen Masterbatch does not contain 6 kinds of objectionable impuritiess such as lead, mercury, cadmium, sexavalent chrome, Polybrominated biphenyl and Poly Brominated Diphenyl Ethers that ROHS bans use of, and the Halogen Masterbatch is used for the conversion of material color.
The present invention---the preparation method that adopts the halogen-free phosphorus-free inflaming retarding polyolefine material of radiation grafting technology preparation is by the material blend of specifying proportioning, extrude, the granulation supervisor constitutes.Specifically, with above-mentioned composite antioxidant, AL (OH)
3With Mg (OH)
2Mixture, zinc borate, divalence metallic soap of stearic acid salt lubricant, the Halogen Masterbatch is successively with 0.5～4 part, 40～80 parts, 10～20 parts, 1～3 part, 0～5 part relative weight, with relative weight be 5～15 parts ethylene-vinyl acetate copolymer (EVA-g-MAH) of radiation grafting maleic anhydride and 65～80 parts ethylene-vinyl acetate copolymer (EVA), 15～20 parts linear low density of polyethylene (LLDPE) [or with relative weight be the ethylene-vinyl acetate copolymer (EVA-g-MAH) of 5～15 radiation grafting maleic anhydride and 60～70 parts ethylene-vinyl acetate copolymer (EVA), 15～20 parts linear low density of polyethylene (LLDPE)], 5～15 parts terpolymer EP rubber (EPDM) twin screw extruder in 100～150 ℃ of intervals behind 500 liters high speed kneader thorough mixing is extruded air-cooled granulation.With the particle of above-mentioned relative weight is polyfunctional monomer (methyl) acrylate or triallyl isocyanurate (TAIC) with 50～100 parts melamine cyanurate MCA, 1～3 part lubricant polyethylene wax and 0～3 part crosslinking coagent again, twin screw extruder in 100～150 ℃ of intervals is extruded again behind 500 liters high speed kneader thorough mixing, and air-cooled granulation gets halogen-free phosphorus-free inflaming retarding polyolefine material.
The present invention has following beneficial effect:
Electric wire or heat-shrinkable tube safety performance with above-mentioned halogen-free phosphorus-free inflaming retarding polyolefine material preparation can detect by VW-1 vertical combustion in the standards such as UL3266 and UL224.
Embodiment:
Further specify the present invention with embodiment below, but the present invention is not limited.
Embodiment 1
Commercially available maleic anhydride 3～4kg is dissolved in 6～8kg acetone, again with 100kg ethylene-vinyl acetate copolymer (EVA) after high-speed mixer mixes, after acetone volatilization, again through 100～150 ℃ twin screw extruder granulation, after the rumbatron electron rays or
60Radiation 10～25KGy dosage in the gamma-rays of Co source, the EVA-g-MAH of percentage of grafting 1～1.5%.
Embodiment 2
With the EVA-g-MAH8～12kg of above-mentioned preparation and commercially available composite antioxidant 1～3kg, divalence metallic soap of stearic acid salt 1.5～2.5kg, blue Masterbatch 2～4kg, AL (OH)
3With Mg (OH)
2Mixture 50～75kg, zinc borate 12～18kg, ethylene-vinyl acetate copolymer (EVA) 68～78kg, linear low density of polyethylene (LLDPE) 16～18kg[or with ethylene-vinyl acetate copolymer (EVA) 62～68kg, linear low density of polyethylene (LLDPE) 16～18kg, terpolymer EP rubber (EPDM) 8～12kg] behind 500 liters high speed kneader thorough mixing, extrude air-cooled granulation in 100～150 ℃ twin screw extruder.
Described composite antioxidant is a Hinered phenols antioxidant 1,3,5-trimethylammonium-2,4,6-three (3,5-di-tert-butyl-4-hydroxybenzyl) benzene or pentaerythritol ester 0.5kg, the mixture of two kinds of components of thioesters kind antioxidant Tyox B or thio-2 acid (octadecyl ester) 1～2.5kg.
Embodiment 3
With above-mentioned master batch and commercially available melamine cyanurate MCA70～90kg, polyethylene wax 1.5～2.5kg, three-TRIM (TMPTMA) or triallyl isocyanurate (TAIC) 1～2kg extrude in 100～150 ℃ twin screw extruder behind 500 liters high speed kneader thorough mixing, and air-cooled granulation gets colored low-smoke halide-free fireproof composite polyolefine material.
Embodiment 4
Above-mentioned materials is measured through carrying out flame retardant properties behind the radiation crosslinking by UL3266 standard fabrication Cheng Lanse low-smoke halogen-free phosphor-free fire retardant polyolefin electric wire or by UL224 standard fabrication Cheng Lanse non-halogen non-phosphate heat-shrinkable tube again, and the result can be by VW-1 vertical combustion in the UL standard.
Claims (8)
1. halogen-free phosphorus-free inflaming retarding polyolefine material that adopts radiation grafting technology preparation is characterized in that: be made up of following substances in parts by weight:
5～15 parts of the ethylene-vinyl acetate copolymers of radiation grafting maleic anhydride, 65～80 parts of ethylene-vinyl acetate copolymers, 15～20 parts of linear low density of polyethylene (or 5～15 parts of the ethylene-vinyl acetate copolymers of radiation grafting maleic anhydride, 60～70 parts of ethylene-vinyl acetate copolymers, 5～15 parts of terpolymer EP rubbers, 10～20 parts of linear low density of polyethylene), 0.5～4 part of composite antioxidant, 50～100 parts of melamine cyanurates, AL (OH)
3With Mg (OH)
240～80 parts of mixtures (weight proportion 1: 1), 10～20 parts of zinc borates, 1～3 part of divalence metallic soap of stearic acid salt lubricant, 1～3 part of polyethylene wax lubricant, crosslinking coagent is 0～3 part of polyfunctional monomer (methyl) acrylate or a triallyl isocyanurate, 0～5 part of Halogen Masterbatch, described composite antioxidant is made up of the oxidation inhibitor of following weight ratio: Hinered phenols antioxidant: thioesters kind antioxidant=0.5: 1～3.
2. a kind of halogen-free phosphorus-free inflaming retarding polyolefine material that adopts the radiation grafting technology preparation as claimed in claim 1, it is characterized in that: the ethylene-vinyl acetate copolymer material of the maleic anhydride of radiation grafting technology preparation is by being dissolved in 1～5 part maleic anhydride and 100 parts of ethylene-vinyl acetate copolymers in 2～10 parts the acetone after high-speed mixer mixes, Deng the granulation in twin screw extruder of acetone volatilization back, again through the rumbatron electron rays or
60Radiation 5～30KGy dosage in the gamma-rays of Co source, the radiation grafting material of percentage of grafting 0.5～2%.
3. a kind of halogen-free phosphorus-free inflaming retarding polyolefine material that adopts the radiation grafting technology preparation as claimed in claim 1, it is characterized in that: the melting index MI of ethylene-vinyl acetate copolymer is in 2～6g/min scope, and wherein vinyl acetate content is in 14～40% scopes.
4. a kind of halogen-free phosphorus-free inflaming retarding polyolefine material that adopts the radiation grafting technology preparation as claimed in claim 1, it is characterized in that: described Hinered phenols antioxidant means: 1,3,5-trimethylammonium-2,4,6-three (3,5-di-tert-butyl-4-hydroxybenzyl) benzene, 1,1,3-three (2-methyl-4-hydroxyl-5-t-butyl-phenyl) butane, pentaerythritol ester, β-(3,5-di-tert-butyl-4-hydroxy phenyl) propionic acid octadecyl ester.
5. a kind of halogen-free phosphorus-free inflaming retarding polyolefine material that adopts the radiation grafting technology preparation as claimed in claim 1, it is characterized in that: described thioesters kind antioxidant means: Tyox B, thio-2 acid (octadecyl ester), thio-2 acid two (14 ester).
6. a kind of halogen-free phosphorus-free inflaming retarding polyolefine material that adopts the radiation grafting technology preparation as claimed in claim 1, it is characterized in that: the acrylate cross linked auxiliary agent of described polyfunctional monomer (methyl) means: Viscoat 295, three-TRIM, pentaerythritol triacrylate.
7. the described a kind of preparation method who adopts the halogen-free phosphorus-free inflaming retarding polyolefine material of radiation grafting technology preparation of claim 1 is characterized in that comprising the steps: the composite antioxidant with 0.5～4 part, 0～5 part Halogen Masterbatch, 40～80 parts AL (OH)
3With Mg (OH)
2Mixture, 10～20 parts zinc borate, 1～3 part divalence metallic soap of stearic acid salt lubricant, the ethylene-vinyl acetate copolymer of 1～3 part polyethylene wax lubricant and 5～15 parts radiation grafting maleic anhydride and 65～80 parts ethylene-vinyl acetate copolymer, 15～20 parts linear low density of polyethylene, behind 500 liters high speed kneader thorough mixing, extrude for 100～150 ℃ by two valency twin screw extruders again, air-cooled granulation, this particle is polyfunctional monomer (methyl) acrylate or triallyl isocyanurate with 50～100 parts melamine cyanurate and 0～3 part crosslinking coagent again, behind 500 liters high speed kneader thorough mixing, extruded for 100～150 ℃ by two valency twin screw extruders once more, air-cooled granulation gets halogen-free phosphorus-free inflaming retarding polyolefine material.
8. the described a kind of halogen-free phosphorus-free inflaming retarding polyolefine material of radiation grafting technology preparation that adopts of claim 1 can be used for preparing electric wire and thermal contraction casing tube, and it is characterized in that: electric wire prepared therefrom and the thermal contraction casing tube safety performance behind radiation crosslinking can detect by VW-1 vertical combustion in the standards such as UL3266 and UL224.
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