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CN103881229A - High-flame-retardant and halogen-free polyolefin cable material and preparation method thereof - Google Patents

High-flame-retardant and halogen-free polyolefin cable material and preparation method thereof Download PDF

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Publication number
CN103881229A
CN103881229A CN201410103425.5A CN201410103425A CN103881229A CN 103881229 A CN103881229 A CN 103881229A CN 201410103425 A CN201410103425 A CN 201410103425A CN 103881229 A CN103881229 A CN 103881229A
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China
Prior art keywords
parts
mixing
ethylene
free polyolefin
flame retardant
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Pending
Application number
CN201410103425.5A
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Chinese (zh)
Inventor
梁发雄
张翼翔
蕫启殿
莫伟利
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GUANGDONG JUSHI CHEMICAL INDUSTRY Co Ltd
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GUANGDONG JUSHI CHEMICAL INDUSTRY Co Ltd
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Priority to CN201410103425.5A priority Critical patent/CN103881229A/en
Publication of CN103881229A publication Critical patent/CN103881229A/en
Pending legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L23/04—Homopolymers or copolymers of ethene
    • C08L23/08—Copolymers of ethene
    • C08L23/0846—Copolymers of ethene with unsaturated hydrocarbons containing atoms other than carbon or hydrogen
    • C08L23/0853—Ethene vinyl acetate copolymers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00—Mixing; Kneading
    • B29B7/74—Mixing; Kneading using other mixers or combinations of mixers, e.g. of dissimilar mixers ; Plant
    • B29B7/7461—Combinations of dissimilar mixers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00—Mixing; Kneading
    • B29B7/30—Mixing; Kneading continuous, with mechanical mixing or kneading devices
    • B29B7/58—Component parts, details or accessories; Auxiliary operations
    • B29B7/72—Measuring, controlling or regulating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B9/00—Making granules
    • B29B9/12—Making granules characterised by structure or composition
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
    • B29C48/04—Particle-shaped
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
    • B29C48/375—Plasticisers, homogenisers or feeders comprising two or more stages
    • B29C48/39—Plasticisers, homogenisers or feeders comprising two or more stages a first extruder feeding the melt into an intermediate location of a second extruder
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
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    • B29C48/25—Component parts, details or accessories; Auxiliary operations
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    • B29C48/395—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders
    • B29C48/40—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders using two or more parallel screws or at least two parallel non-intermeshing screws, e.g. twin screw extruders
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    • B29C48/911—Cooling
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    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C—CHEMISTRY; METALLURGY
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    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/0008—Organic ingredients according to more than one of the "one dot" groups of C08K5/01 - C08K5/59
    • C08K5/0066—Flame-proofing or flame-retarding additives
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L23/04—Homopolymers or copolymers of ethene
    • C08L23/06—Polyethene
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L23/04—Homopolymers or copolymers of ethene
    • C08L23/08—Copolymers of ethene
    • C08L23/0846—Copolymers of ethene with unsaturated hydrocarbons containing atoms other than carbon or hydrogen
    • C08L23/0869—Copolymers of ethene with unsaturated hydrocarbons containing atoms other than carbon or hydrogen with unsaturated acids, e.g. [meth]acrylic acid; with unsaturated esters, e.g. [meth]acrylic acid esters
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    • C09K21/00—Fireproofing materials
    • C09K21/06—Organic materials
    • C09K21/12—Organic materials containing phosphorus
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
    • H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
    • H01B3/30—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes
    • H01B3/44—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes vinyl resins; acrylic resins
    • H01B3/441—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes vinyl resins; acrylic resins from alkenes
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    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • B29B7/02—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type
    • B29B7/06—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type with movable mixing or kneading devices
    • B29B7/10—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type with movable mixing or kneading devices rotary
    • B29B7/18—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type with movable mixing or kneading devices rotary with more than one shaft
    • B29B7/183—Mixing; Kneading non-continuous, with mechanical mixing or kneading devices, i.e. batch type with movable mixing or kneading devices rotary with more than one shaft having a casing closely surrounding the rotors, e.g. of Banbury type
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    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B7/00—Mixing; Kneading
    • B29B7/30—Mixing; Kneading continuous, with mechanical mixing or kneading devices
    • B29B7/34—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices
    • B29B7/38—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices rotary
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    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
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    • B29B7/30—Mixing; Kneading continuous, with mechanical mixing or kneading devices
    • B29B7/34—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices
    • B29B7/38—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices rotary
    • B29B7/46—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices rotary with more than one shaft
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • B29B9/02—Making granules by dividing preformed material
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Abstract

The invention discloses a high-flame-retardant and halogen-free polyolefin cable material and a preparation method thereof. The high-flame-retardant and halogen-free polyolefin cable material comprises the following components in parts by weight: 20-70 parts of ethylene copolymer, 5-30 parts of polyethylene, 10-60 parts of metal hydroxide, 3-20 parts of organic phosphate flame retardant, 3-30 parts of melamine compound, 4-10 parts of compatilizer and 2-5 of other additives. The preparation method comprises the following steps of: (1) firstly putting granular materials into a high-speed mixing machine, adding liquid additive after stirring for 30 seconds at low speed, mixing for 3 minutes at high speed, then stopping, adding the granular materials, mixing for 3 minutes at high speed, then stopping and obtaining premixed materials; and (2) adding the premixed materials into a mixer for mixing for 15 minutes, then mixing by double screws with same directions, finally extruding by single screw, carrying out air cooling, hot cutting and granulation, wherein the extruding temperature is set between 90-130 DEG C.

Description

A kind of high flame retardant halogen-free polyolefin CABLE MATERIALS and preparation method thereof
Technical field
The present invention relates to a kind of non-halogen flame-retardant cable, refer in particular to a kind of high flame retardant halogen-free polyolefin CABLE MATERIALS and preparation method thereof.
Background technology
Along with rapid development of economy, electric wire is used widely in every profession and trade, and along with the frequent generation of appliance fire accident, the fire-retardant problem of electric wire has caused the attention of countries in the world.Traditional fire-resistant cable material mainly adopts PVC and adds the polyolefine of halogen-antimony fire retardant, discharges a large amount of smog and toxic gas when cable fire, has hindered people's safe escape and fire-fighting work in fire, makes lives and properties suffer heavy losses.
European Union's dependent instructions such as RoHS instruction, WEEE instruction, REACH instruction and EuP instruction that release one after another in recent years, the electric wire product that EuP command request enters EU market must meet Halogen-free requirement, thereby the high flame retardant halogen-free polyolefin CABLE MATERIALS with self-extinguishing become the direction of electric wire and cable material development, future develop is open.
In prior art, people conventionally adopt following two kinds of methods to prepare non-halogen flame-retardant cable: the first, and inorganic combustion inhibitor aluminium hydroxide (ATH), magnesium hydroxide (MH), zinc borate add to prepares non-halogen flame-retardant cable in matrix; The second, adopt antimonous oxide and metal hydroxides to prepare non-halogen flame-retardant cable.The product flame retarding efficiency that uses first method to prepare is low, reach good flame retardant effect, and inorganic combustion inhibitor addition is more than at least 65%, and a large amount of weighting materials causes CABLE MATERIALS physical and mechanical properties, electric property and processing characteristics to worsen; The product that uses second method to prepare, can require to add antimonous oxide for meeting Flame Retardancy, the CABLE MATERIALS that contains antimonous oxide can discharge a large amount of obnoxious flavoures in the time of burning, cause environmental pollution and human injury, Huawei and three magnitude producers have banned use of the material containing antimonous oxide at present.
Summary of the invention
The object of the invention is by adopting organic hypophosphite, melamine compound and metal hydroxides composite preparation high flame retardant halogen-free polyolefin CABLE MATERIALS; And provide a kind of preparation method of above-mentioned high flame retardant halogen-free polyolefin CABLE MATERIALS.
The present invention realizes by the following technical solutions:
A kind of high flame retardant halogen-free polyolefin CABLE MATERIALS, comprise the component of following parts by weight proportioning, 20～70 parts of ethylene copolymers, 5～30 parts of polyethylene, 10～60 parts of metal hydroxidess, 3～20 parts of organophosphate fire retardants, 3～30 parts of melamine compounds, 4～10 parts of compatilizers, 2～5 parts of other auxiliary agents; Wherein, described ethylene copolymer is ethylene-methyl acrylate multipolymer, ethylene-ethyl acrylate multipolymer, ethylene-butyl acrylate multipolymer, ethylene-vinyl acetate copolymer; Described metal hydroxides is one or both the mixture in aluminium hydroxide and magnesium hydroxide; Described organic hypophosphite fire retardant is one or more the mixture in methyl hypo-aluminum orthophosphate, methylethyl hypo-aluminum orthophosphate, phenyl hypo-aluminum orthophosphate, diethyl hypo-aluminum orthophosphate, diethyl zinc hypophosphite, methylethyl zinc hypophosphite, cyclohexyl zinc hypophosphite, phenyl zinc hypophosphite fire retardant.
In addition, described polyethylene is one or more the mixture in Low Density Polyethylene, linear low density polyethylene, high density polyethylene(HDPE), metallocene PE.Described melamine compound is one or more the mixture in melamine cyanurate, melamine phosphate, melamine pyrophosphate, boric acid trimeric cyanamide, polyphosphoric acid melamine.Described compatilizer is one or more the mixture in maleic anhydride grafted ethene-octene copolymer, maleic anhydride graft styrene series elastomer, maleic anhydride grafted ethene-methyl acrylate copolymer, maleic anhydride grafted linear low density polyethylene, maleic anhydride grafted ethene-acetate ethylene copolymer.Described other auxiliary agent is one or more the mixture in antioxidant, lubricant, coupling agent, toner pigment, these auxiliary agents be commercial product and in the industry by those of ordinary skill is known, thereby just do not enumerate at this.
The preparation method who the invention allows for above-mentioned high flame retardant halogen-free polyolefin CABLE MATERIALS, comprises the steps:
(1) after each component is accurately weighed by formula, mix after 6 minutes and obtain Preblend in high-speed mixer, concrete steps are as follows, first granular feedstock dropped in high-speed mixer, add liquid adjuvants high-speed mixing shut down after 3 minutes in stirring at low speed after 30 seconds; Add afterwards powder raw material high-speed mixing to shut down after 3 minutes, obtain Preblend;
(2) add mixer mixing after 15 minutes above-mentioned Preblend, more mixing through parallel dual-screw, finally by the air-cooled fervent granulation of single Screw Extrusion, extrusion temperature is set as between 90～130 ℃.
The present invention compared with prior art, by preferred high strength ethylene-vinyl acetate copolymer and metallocene PE resin alloy, improves material compatibility with interpolation compatilizer, and tensile strength of material is greater than 12MPa, and elongation at break is greater than 200%.
The present invention also selects organic hypophosphite fire retardant as becoming charcoal promotor, and at condensed phase performance fire retardation, in combustion processes, it can accelerate resin and be dehydrated into charcoal; Itself and trimeric cyanamide chemical combination and aluminium hydroxide use jointly, and material self-extinguishing is good, and the amount of being fuming is little, and oxygen index is greater than 50, and finished product electric wire is fire-retardant simultaneously meets IEC60332-1 and UL1581VW-1 requirement.
The present invention carries out mixing granulator with Banbury mixer and twin-screw extrusion board in preparation process, and independent research special screw thread element and combination guarantee the abundant mixing dispersion of each component in formula, and material mechanical performance is good, extrudes electric wire smooth surface.
In a word, product produced according to the invention, density is lower than similar high flame-retardant cable product, and cost performance is high, and not halogen-containing, antimonous oxide, red phosphorus, and mechanical property is superior, and flame retardant properties is good, meets the requirement of international standard and GB.
Embodiment
Base case of the present invention is to having shown a kind of high flame retardant halogen-free polyolefin CABLE MATERIALS, comprise the component of following parts by weight proportioning, 20～70 parts of ethylene copolymers, 5～30 parts of polyethylene, 10～60 parts of metal hydroxidess, 3～20 parts of organophosphate fire retardants, 3～30 parts of melamine compounds, 4～10 parts of compatilizers, 2～5 parts of other auxiliary agents; Wherein, described ethylene copolymer is ethylene-methyl acrylate multipolymer, ethylene-ethyl acrylate multipolymer, ethylene-butyl acrylate multipolymer, ethylene-vinyl acetate copolymer; Described metal hydroxides is one or both the mixture in aluminium hydroxide and magnesium hydroxide; Described organic hypophosphite fire retardant is one or more the mixture in methyl hypo-aluminum orthophosphate, methylethyl hypo-aluminum orthophosphate, phenyl hypo-aluminum orthophosphate, diethyl hypo-aluminum orthophosphate, diethyl zinc hypophosphite, methylethyl zinc hypophosphite, cyclohexyl zinc hypophosphite, phenyl zinc hypophosphite fire retardant.
In addition, described polyethylene is one or more the mixture in Low Density Polyethylene, linear low density polyethylene, high density polyethylene(HDPE), metallocene PE.Described melamine compound is one or more the mixture in melamine cyanurate, melamine phosphate, melamine pyrophosphate, boric acid trimeric cyanamide, polyphosphoric acid melamine.Described compatilizer is one or more the mixture in maleic anhydride grafted ethene-octene copolymer, maleic anhydride graft styrene series elastomer, maleic anhydride grafted ethene-methyl acrylate copolymer, maleic anhydride grafted linear low density polyethylene, maleic anhydride grafted ethene-acetate ethylene copolymer.Described other auxiliary agent is one or more the mixture in antioxidant, lubricant, coupling agent, toner pigment, these auxiliary agents be commercial product and in the industry by those of ordinary skill is known, thereby only in embodiment, suitably select (being that the auxiliary agent that performance is identical and close can be replaced mutually according to practical situation), just do not enumerate at this.
The present invention returns the preparation method who has shown above-mentioned high flame retardant halogen-free polyolefin CABLE MATERIALS, comprises the steps:
(1) after each component is accurately weighed by formula, mix after 6 minutes and obtain Preblend in high-speed mixer, concrete steps are as follows, first granular feedstock dropped in high-speed mixer, add liquid adjuvants high-speed mixing shut down after 3 minutes in stirring at low speed after 30 seconds; Add afterwards powder raw material high-speed mixing to shut down after 3 minutes, obtain Preblend;
(2) add mixer mixing after 15 minutes above-mentioned Preblend, more mixing through parallel dual-screw, finally by the air-cooled fervent granulation of single Screw Extrusion, extrusion temperature is set as between 90～130 ℃.
Below in conjunction with embodiment, the invention will be further described.
As shown in table 1, in table, provide formula and the proportion of composing thereof of embodiment 1-10.
Pressing proportioning shown in table 1 presses each component after the accurate weighing of formula, in high-speed mixer, mix after 6 minutes and obtain Preblend, concrete steps are as follows, first granular feedstock dropped in high-speed mixer, add liquid adjuvants high-speed mixing shut down after 3 minutes in stirring at low speed after 30 seconds; Add afterwards powder raw material high-speed mixing to shut down after 3 minutes, obtain Preblend.
Add mixer mixing after 15 minutes above-mentioned Preblend, more mixing through parallel dual-screw, finally by the air-cooled fervent granulation of single Screw Extrusion, extrusion temperature is set as between 90～130 ℃.
The test piece of above-described embodiment sample adopts compression molding preparation, be to plastify slice in two roller mills of 100～130 ℃ in temperature by pellet, be mold pressing test sample on the vulcanizing press of 165～180 ℃ in temperature again, gained properties of sample testing method is as follows: (1) density: carry out according to ASTM D792 standard; (2) tensile property: carry out draw speed 200 ± 50mm/min, respectively test tensile strength, elongation at break according to ISO527-3 standard; (3) aging back draft performance: standard batten is put into ventilation ageing test box and carry out 121 ℃, heat-proof aging test in 168 hours, after batten takes out, constant temperature was tested tensile property after 24 hours, and testing standard is undertaken by ISO527-3 standard; (4) electric property: according to 20 of IEC60093 test material ℃ of volume specific resistances; According to the dielectric strength of IEC60243-1 test material; (5) flame retardant properties: according to the oxygen index of ISO4589 test material (OI); According to UL94V-0 standard testing 3.0mm standard batten flame retardant properties.(6) combustionproperty: according to ASTM E622 test material smoke density; While burning according to IEC60754-1 test material, discharge total amount of halogen acid gas; While measuring material combustion according to IEC60754-2, discharge the acidity of gas; By Φ 50PVC electric wire forcing machine, processing temperature is between 140～160 ℃, and above-mentioned materials is made to wire diameter 2.0mm electric wire on this basis, wall thickness 0.35mm, and standard copper wire specification is 0.12 × 20, according to UL1581 test wires VW-1 combustion case.
Embodiment 1-3 formula, adopts respectively ethylene-vinyl acetate copolymer, ethylene-methyl acrylate multipolymer, three kinds of different polyolefin resines of ethylene-ethyl acrylate multipolymer, and all the other components and ratio all remain unchanged.The performance test results shows: gained properties of sample all meets every service requirements, and tensile strength is all greater than 12MPa, and elongation at break is greater than 200%, and oxygen index is greater than 50.Wherein the tensile strength of sample 1 and elongation at break are all best.
Embodiment 4 fills a prescription and on the basis of embodiment 1, only changes fire retardant proportioning, and all the other components and ratio all remain unchanged.The performance test results shows: compared with sample 1, by the increase of organic hypophosphite fire retardant ratio, sample flame retardant properties improves, and mechanical property declines to some extent, but still can meet every service requirements.
Embodiment 5, on the basis of embodiment 1, reduces metallocene ethene addition, increases aluminium hydroxide addition, and all the other each component ratios all remain unchanged.Test result shows: compared with sample 1, by the increase of aluminium hydroxide fire retardant ratio, sample flame retardant properties improves, and smoke density reduces, and mechanical property declines to some extent, but still can meet every service requirements.
Embodiment 6, on the basis of embodiment 5, reduces melamine cyanurate addition, increases aluminium hydroxide addition, and all the other each component ratios all remain unchanged.Test result shows: compared with sample 5, by the increase of aluminium hydroxide fire retardant ratio, sample flame retardant properties is substantially constant, and smoke density reduces, and mechanical property slightly rises, and properties of sample meets every service requirements.
Embodiment 7, on the basis of embodiment 5, adopts polyphosphoric acid melamine equivalent to replace melamine cyanurate, and all the other each component ratios all remain unchanged.Compared with sample 5, sample flame retardant properties slightly rises, and mechanical properties decrease is obvious, but still can meet every service requirements.
Embodiment 8, on the basis of embodiment 7, only changes fire retardant proportioning, and all the other each component ratios all remain unchanged.Compared with sample 7, reduce polyphosphoric acid melamine addition, increase melamine cyanurate addition, fire retardant total addition level remains unchanged, and the impact of sample flame retardant properties is little, and mechanical property rises, and properties of sample meets every service requirements.
Table 1
Figure BDA0000478795470000061
Embodiment 9, on the basis of embodiment 8, only changes fire retardant proportioning, and all the other each component ratios all remain unchanged.Compared with sample 8, reduce organic hypophosphite addition, increase aluminium hydroxide addition, fire retardant total addition level remains unchanged, and sample smoke density reduces, and flame retardant properties declines, but still can test by UL1581VW-1.
Embodiment 10, on the basis of embodiment 8, increases ethylene-vinyl acetate copolymer addition, reduces compatilizer addition, and all the other each component ratios all remain unchanged.Compared with sample 8, reduce compatilizer addition, sample tensile strength reduces, and elongation at break increases, and flame retardant properties is substantially constant, and properties of sample meets every service requirements.
Provide four groups of comparative examples below.Formula and the proportion of composing thereof of comparative example 11-13 are as shown in table 2.
Table 2
Figure BDA0000478795470000071
Figure BDA0000478795470000081
Comparative example 11, on the basis of embodiment 1, only changes fire retardant type, substitutes organic hypophosphite fire retardant system with antimonous oxide system, and all the other each component ratios remain unchanged.Test result shows: sample 11 good mechanical properties, and fire retardant total addition level remains unchanged, and sample oxygen index reduces, and smoke density increases, and electric wire VW-1 test is not passed through.
Comparative example 12, on the basis of embodiment 1, reduces aluminium hydroxide addition, increases nitrogen phosphorus composite flame-retardant agent addition, and all the other each component ratios remain unchanged.Test result shows: sample 12 mechanical properties decrease are serious, and fire retardant total addition level remains unchanged, and the amount of being fuming obviously increases.
Comparative example 13, on the basis of embodiment 5, fire retardant total amount is constant, changes fire retardant type and proportioning, and all the other each component ratios all remain unchanged.Compared with sample 5, use aluminium hydroxide, magnesium hydroxide, zinc borate flame retardant, sample oxygen index reduces, and electric wire VW-1 test is not passed through.
Comparative example 14, on the basis of embodiment 10, reduces metallocene PE addition, increases fire retardant addition, and all the other each component ratios all remain unchanged.Compared with sample 10, use separately flame retardant of magnesium hydroxide, fire retardant total addition level increases, and sample 13 mechanical properties decrease are serious, and electric wire VW-1 test is not passed through.
According to the elaboration in above specification sheets, those skilled in the art in the invention can also carry out suitable change and modification to above-mentioned embodiment.Therefore, the content of mentioning in above-described embodiment is not limitation of the invention, is not departing under the prerequisite of inventive concept of the present invention, and any apparent replacement is all within protection scope of the present invention.

Claims (6)

1. a high flame retardant halogen-free polyolefin CABLE MATERIALS, comprises the component of following parts by weight proportioning,
20～70 parts of ethylene copolymers, 5～30 parts of polyethylene, 10～60 parts of metal hydroxidess, 3～20 parts of organophosphate fire retardants, 3～30 parts of melamine compounds, 4～10 parts of compatilizers, 2～5 parts of other auxiliary agents;
Wherein, described ethylene copolymer is the one of ethylene-methyl acrylate multipolymer, ethylene-ethyl acrylate multipolymer, ethylene-butyl acrylate multipolymer or ethylene-vinyl acetate copolymer; Described metal hydroxides is one or both the mixture in aluminium hydroxide and magnesium hydroxide; Described organic hypophosphite fire retardant is one or more the mixture in methyl hypo-aluminum orthophosphate, methylethyl hypo-aluminum orthophosphate, phenyl hypo-aluminum orthophosphate, diethyl hypo-aluminum orthophosphate, diethyl zinc hypophosphite, methylethyl zinc hypophosphite, cyclohexyl zinc hypophosphite, phenyl zinc hypophosphite fire retardant.
2. high flame retardant halogen-free polyolefin CABLE MATERIALS according to claim 1, is characterized in that: described polyethylene is one or more the mixture in Low Density Polyethylene, linear low density polyethylene, high density polyethylene(HDPE), metallocene PE.
3. high flame retardant halogen-free polyolefin CABLE MATERIALS according to claim 1, is characterized in that: described melamine compound is one or more the mixture in melamine cyanurate, melamine phosphate, melamine pyrophosphate, boric acid trimeric cyanamide, polyphosphoric acid melamine.
4. high flame retardant halogen-free polyolefin CABLE MATERIALS according to claim 1, is characterized in that: described compatilizer is one or more the mixture in maleic anhydride grafted ethene-octene copolymer, maleic anhydride graft styrene series elastomer, maleic anhydride grafted ethene-methyl acrylate copolymer, maleic anhydride grafted linear low density polyethylene, maleic anhydride grafted ethene-acetate ethylene copolymer.
5. high flame retardant halogen-free polyolefin CABLE MATERIALS according to claim 1, is characterized in that: described other auxiliary agent is one or more the mixture in antioxidant, lubricant, coupling agent, toner pigment.
6. a preparation method for high flame retardant halogen-free polyolefin CABLE MATERIALS as claimed in claim 1, is characterized in that comprising the steps:
(1) after each component is accurately weighed by formula, mix after 6 minutes and obtain Preblend in high-speed mixer, concrete steps are as follows, first granular feedstock dropped in high-speed mixer, add liquid adjuvants high-speed mixing shut down after 3 minutes in stirring at low speed after 30 seconds; Add afterwards powder raw material high-speed mixing to shut down after 3 minutes, obtain Preblend;
(2) add mixer mixing after 15 minutes above-mentioned Preblend, more mixing through parallel dual-screw, finally by the air-cooled fervent granulation of single Screw Extrusion, extrusion temperature is set as between 90～130 ℃.
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Application publication date: 20140625