CN101906226A - Conductive and antiflaming ethylene-vinyl acetate composite material with low smoke and preparation method thereof - Google Patents
Conductive and antiflaming ethylene-vinyl acetate composite material with low smoke and preparation method thereof Download PDFInfo
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- CN101906226A CN101906226A CN 201010248018 CN201010248018A CN101906226A CN 101906226 A CN101906226 A CN 101906226A CN 201010248018 CN201010248018 CN 201010248018 CN 201010248018 A CN201010248018 A CN 201010248018A CN 101906226 A CN101906226 A CN 101906226A
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Abstract
The invention provides a conductive and antiflaming ethylene-vinyl acetate composite material with low smoke and a preparation method thereof, belonging to the technical field of high molecule composite materials. Fillers are uniformly dispersed in an ethylene-vinyl acetate base body through a macro molecule melting intercalation method by taking ethylene-vinyl acetate as the base body and taking conductive carbon blacks and palygorskite clays as the fillers. Through the means of electronic microscope scanning, thermogravimetric analysis, a horizontal and vertical combustion apparatus, an oxygen index apparatus, a semi-conduction rubber and plastic resistance tester and a smoke density tester, and the like, the detection shows that the prepared ethylene-vinyl acetate composite material has excellent conductivity, antiflaming property, lower smoke density value, reduced fused mass dripping speed, reduced flame intensity and prolonged ignition time, and satisfies the application index and the requirement of the material in the industrial field of electric wires and cables.
Description
Technical field
The invention belongs to polymeric material field, relate to a kind of polymer composite, relate in particular to a kind of ethylene-vinyl acetate composite material, be mainly used in cable industry with conduction flame retardant properties.The invention still further relates to the preparation method of this ethylene-vinyl acetate composite material.
Background technology
The composite polymer electro-conductive material comes down to a kind of polymer composite with conductivity, typically refer to the macromolecular material is matrix, add various materials with conductive capability, mainly be some mineral fillers, pass through modes such as dispersion is compound, lamination is compound and handle the heterogeneous compound system that afterwards has conducting function.Composite polymer electro-conductive material and structural conductive polymer phase ratio, has the advantage that processing is simple, cost is low, and combine the characteristic of each component, the electroconductibility that had both had filler, the various excellent specific properties that have macromolecular material again, can regulate the electric property and the mechanical property of material according to the actual requirements on a large scale, easy to use.Therefore, it is weaved at light industry, the energy, and electronics, fields such as aerospace have obtained developing rapidly and widespread use.Along with the modernization of science and technology and developing rapidly of electronic industry, the demand of this type material can be increasing.Conductive polymer composites can be divided into conductive rubber according to the difference of matrix, conductive plastics, electro-conductive fiber, electroconductive binder.According to the difference of material function, can be divided into anti-electrostatic and destatic material, electrode materials, exothermic material, electromagnetic shielding material etc.
Ethylene-vinyl acetate (EVA) is development in recent years one of plastics variety rapidly, and it has good shock-resistance, snappiness, environmental stress crack resistance, with filler, fire retardant compatibility is preferably arranged simultaneously.Multiple processing modes such as EVA is suitable for extruding, injection, blowing, thermoforming, the production main products has multiclass products such as tubing, sheet material, building materials, electric fittings, cable insulation material and daily necessities.But EVA is the same with polyolefine inflammable, produce the black smoke have poisonous gas simultaneously, limited its in side such as household electrical appliances, building, building materials, cable insulation and application, so aborning, the flame-proof smoke-suppressing of EVA more and more causes people's attention.With the cable industry is example, and cable is harsh day by day to the requirement of the flame-proof smoke-suppressing and the feature of environmental protection.The requirement of polymkeric substance is promptly wanted can flame-retardant smoke inhibition, also will meet electrical property and mechanical property requirements.Therefore, be matrix with ethylene-vinyl acetate (EVA), compound filler with conductivity prepares a kind of ethylene-vinyl acetate composite material with conduction flame retardant properties, has crucial meaning.
In many conductive filler materials, carbon black is the widest a kind of of consumption maximum, range of application.Carbon black is as a kind of nano material, not only raw material abundance, low price, stable conductivity, but also have nano level particle diameter (can reach the 10nm magnitude), carbon black also has good painted and strengthening action simultaneously.In addition, the development of off-colour industry is also fairly perfect, and the selective and use of kind of carbon black of various trade mark is arranged.Therefore, the multiple factors such as price, electric property and stability of comprehensive filler, graphitized carbon black is more satisfactory a kind of conductive filler material, also is to use maximum a kind of conductive filler materials in research and the production.
Polygorskite is the abundant valuable sources that remain to be developed of the western reserves of China.It is the micropore of 0.32 * 0.73nm that the aperture consistent with its length direction arranged in the polygorskite crystal, the hole contains a large amount of ignition-proof element magnesium, aluminium and water of different nature, as crystal water, hydroxyl structure water, zeolite molecules water and inclusion water etc., the water vapour that these water at high temperature produce is favourable to phosphorus flame retardant especially, and the porous of polygorskite and hollow structure have strong adsorption to gas, and the heat insulation thermal insulation of hollow can be blocked the transmission of heat, and these characteristics make it have good flame retardancy.Simultaneously polygorskite have non-volatile, cheap, have concurrently fire-retardant, press down cigarette and reduce the function of toxic gas, so be the nuisanceless fire retardant of ideal.
Summary of the invention
The purpose of this invention is to provide a kind of conduction antiflaming ethylene-vinyl acetate composite material with low smoke.
Another object of the present invention provides a kind of preparation method of conducting electricity antiflaming ethylene-vinyl acetate composite material with low smoke.
Conduction antiflaming ethylene-vinyl acetate composite material with low smoke of the present invention is to be matrix with the ethylene-vinyl acetate, is filler with graphitized carbon black and polygorskite, by the macromole melt intercalated method, uniform filling is dispersed in the ethylene-vinyl acetate matrix.
The mass ratio of described ethylene-vinyl acetate and filler is 1: 0.1～1: 0.5; In the described filler, the mass ratio of graphitized carbon black and polygorskite is 1: 1～1: 0.1.
The preparation method of antiflaming ethylene-vinyl acetate composite material with low smoke is conducted electricity in the present invention, be with the ethylene-vinyl acetate particle in 40～70 ℃ of following vacuum-drying 24～48h, place on the two roll plastic mixing mill heating and melting to flowing; The graphitized carbon black and the polygorskite filler (mass ratio of graphitized carbon black and polygorskite is 1: 1～1: 0.1) that add 0.1～0.5 times of ethylene-vinyl acetate granular mass, mixing 0.1～0.4 hour in 110～150 ℃, place on the vulcanizing press then, in 110～150 ℃, compression moulding under 8～10Mpa.
When adding filler, add ethylene-vinyl acetate granular mass 3.0 * 10
-3～5 * 10
-3Antioxidant doubly also can add doubly 0.01～0.03 lubricant of ethylene-vinyl acetate granular mass.
The antioxidant that the present invention adopts has 2,2-methylene-bis (4-methyl-6-tert butyl phenol), (3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid pentaerythritol ester, triphenyl phosphite etc.; Lubricant has ethylene group two hard esteramides (EBS), glyceryl monostearate (GMS) or Tristearoylglycerols (HTG).
The conductive carbon black that the present invention adds has acetylene carbon black (as N220, N330, N339, N550, N660, MT), paint, printing ink ordinary carbon black (R400R) and superconduction carbon black (VXC-72).
Below by means such as infrared spectrum, electron-microscope scanning, thermogravimetric analysis and vertical combustion instrument, smoke density instrument, structure, the performance of the ethylene-vinyl acetate composite material of the present invention preparation elaborated.
1, electron-microscope scanning
Fig. 1 is the electron-microscope scanning figure of ethylene-vinyl acetate composite material of the present invention.From Fig. 1 we as can be seen, carbon black and palygorskite clay have certain agglomeration in matrix, but whole disperse more even.
2, thermogravimetric analysis
Fig. 2 is the thermogravimetric curve of ethylene-vinyl acetate composite material of the present invention.Curve a wherein, b are matrix material thermogravimetric curve (its difference is the contained filler percentage composition of matrix material difference); C is pure ethylene-vinyl acetate thermogravimetric curve.By thermal multigraph as can be seen, matrix material pure relatively matrix of thermostability between 350 ℃～450 ℃ increases, and after 500 ℃, the matrix material thermal weight loss tends towards stability, and the pure relatively matrix of remaining carbon is higher.
3, conductivity
3.1 testing tool: semiconduction rubber and plastic resistance meter
3.2 making sample: each three on the sample that in test piece, intercepts both direction in length and breadth with the punch die machine.Sample is the rectangle test piece, length 110mm, width 50mm, thickness 2mm or 4mm.Thickness should be got its mean value along 6 calculating of the roughly equidistant measurement of test piece length, the survey of every bit be worth most difference with mean value should be no more than+5%.
3.3 testing standard environment and requirement: 25 ℃ of temperature, relative humidity 50%;
3.4 test result: every sample is surveyed six times, asks its data mean value, asks the mean value of every all sample datas of test piece then.Resistivity is in 0.7～45 Ω cm scope.
4, smoke density test
4.1 testing tool: JSC-1 type smoke density tester
4.2 making sample: in each test piece, intercept each five on sample, specimen length 75mm, width 75mm, thickness 1mm with the punch die machine.Specimen surface is smooth, thickness is even, defectives such as non-trimming and burr.
4.3 testing standard environment and requirement: before test, it is 50% environment 40h that sample is placed 25 ℃, relative humidity.
4.4 test result: reject maximum value and minimum value, get the mean value of three tests.The smoke density value is 100～150.
5, flame retardant properties test
5.1 testing tool: JF-4 type limiting oxygen index determination instrument
5.2 making sample: in each test piece, intercept sample with the punch die machine.Every group of sample intercepts 5, and its batten specification is: length 150mm, width 6mm, thickness 3mm.Specimen surface is smooth, thickness is even, defectives such as non-trimming and bubble.
5.3 test result: oxygen index is 28.0～31.2.
To sum up experimental result shows, the ethylene-vinyl acetate composite material of the present invention's preparation, have and excellent conducting performance, flame retardant properties and lower smoke density value, the melt dropleting speed reduces, flame intensity reduces, and burning time prolongs, and has satisfied application indexes and the requirement of this material at the electric wire industrial circle.
Description of drawings
Fig. 1 is the electron-microscope scanning figure of ethylene-vinyl acetate composite material of the present invention
Fig. 2 is the thermogravimetric curve of ethylene-vinyl acetate composite material of the present invention.
Embodiment
Embodiment 1: the ethylene-vinyl acetate particle is placed loft drier, in 70 ℃ of following vacuum-drying 48h, forward on the two roll plastic mixing mill heating and melting then to flowing; The graphitized carbon black and the polygorskite filler (mass ratio of graphitized carbon black and polygorskite is 1: 1) that add 0.43 times of ethylene-vinyl acetate granular mass, ethylene-vinyl acetate granular mass 3.0 * 10
-3Antioxidant 2 doubly, the lubricant EBS that 2-methylene-bis (4-methyl-6-tert butyl phenol) and ethylene-vinyl acetate granular mass are 0.01 times, mixing 7 minutes in 115 ℃.After fully mixing, material is taken off from rod, place on the vulcanizing press, in 115 ℃, compression moulding under the 10Mpa.Material is taken out, make the sample of desired shape, to be measured.
After measured, its resistivity is 4.495 Ω cm, and the smoke density value is 108, and oxygen index is 28.8.
Embodiment 2: the ethylene-vinyl acetate particle is placed loft drier, in 70 ℃ of following vacuum-drying 48h, forward on the two roll plastic mixing mill heating and melting then to flowing; The graphitized carbon black and the polygorskite filler (mass ratio of graphitized carbon black and polygorskite is 3: 1) that add 0.43 times of ethylene-vinyl acetate granular mass, ethylene-vinyl acetate granular mass 3.5 * 10
-3The lubricant EBS that antioxidant triphenyl phosphite doubly and ethylene-vinyl acetate granular mass are 0.01 times.Mixing 10 minutes in 120 ℃.After fully mixing, material is taken off from rod, place on the vulcanizing press, in 120 ℃, compression moulding under the 10Mpa.Material is taken out, make the sample of desired shape, to be measured.
After measured, its resistivity is 1.981 Ω cm, and the smoke density value is 114, and oxygen index is 30.9.
Embodiment 3: the ethylene-vinyl acetate particle is placed loft drier, in 70 ℃ of following vacuum-drying 48h, forward on the two roll plastic mixing mill heating and melting then to flowing; The graphitized carbon black and the polygorskite filler (mass ratio of graphitized carbon black and polygorskite is 5: 1) that add 0.40 times of ethylene-vinyl acetate granular mass, ethylene-vinyl acetate granular mass 3.8 * 10
-3Antioxidant triphenyl phosphite doubly, the lubricant EBT that the ethylene-vinyl acetate granular mass is 0.015 times.Mixing 10 minutes in 120 ℃.After fully mixing, material is taken off from rod, place on the vulcanizing press, in 125 ℃, compression moulding under the 10Mpa.Material is taken out, make the sample of desired shape, to be measured.
After measured, its resistivity is 1.124 Ω cm, and the smoke density value is 120, and oxygen index is 28.2.
Embodiment 4: the ethylene-vinyl acetate particle is placed loft drier, in 70 ℃ of following vacuum-drying 48h, forward on the two roll plastic mixing mill heating and melting then to flowing; The graphitized carbon black and the polygorskite filler (mass ratio of graphitized carbon black and polygorskite is 4: 1) that add 0.33 times of ethylene-vinyl acetate granular mass, ethylene-vinyl acetate granular mass 4.0 * 10
-3Antioxidant 2 doubly, the lubricant Tristearoylglycerol (HTG) that 2-methylene-bis (4-methyl-6-tert butyl phenol) and ethylene-vinyl acetate granular mass are 0.116 times.Mixing 15 hours in 125 ℃.After fully mixing, material is taken off from rod, place on the vulcanizing press, in 120 ℃, compression moulding under the 10Mpa.Material is taken out, make the sample of desired shape, to be measured.
After measured, its resistivity is 0.943 Ω cm, and the smoke density value is 113, and fire burning index is 28.
Embodiment 5: the ethylene-vinyl acetate particle is placed loft drier, in 70 ℃ of following vacuum-drying 48h, forward on the two roll plastic mixing mill heating and melting then to flowing; The graphitized carbon black and the polygorskite filler (mass ratio of graphitized carbon black and polygorskite is 5: 1) that add 0.3 times of ethylene-vinyl acetate granular mass, ethylene-vinyl acetate granular mass 4 * 10
-3Antioxidant 2 doubly, the two hard esteramides (EBS) of the lubricant ethylene group that 2-methylene-bis (4-methyl-6-tert butyl phenol) and ethylene-vinyl acetate granular mass are 0.02 times.Mixing 15 minutes in 120 ℃.After fully mixing, material is taken off from rod, place on the vulcanizing press, in 120 ℃, compression moulding under the 10Mpa.Material is taken out, make the sample of desired shape, to be measured.
After measured, its resistivity is 0.723 Ω cm, and the smoke density value is 129, and oxygen index is 29.3.
Embodiment 6: the ethylene-vinyl acetate particle is placed loft drier, in 60 ℃ of following vacuum-drying 48h, forward on the two roll plastic mixing mill heating and melting then to flowing; The graphitized carbon black and the polygorskite filler (mass ratio of graphitized carbon black and polygorskite is 5: 1) that add 0.35 times of ethylene-vinyl acetate granular mass, ethylene-vinyl acetate granular mass 4.5 * 10
-3Antioxidant 2 doubly, the two hard esteramides (EBS) of the lubricant ethylene group that 2-methylene-bis (4-methyl-6-tert butyl phenol) and ethylene-vinyl acetate granular mass are 0.03 times.Mixing 25 minutes in 150 ℃.After fully mixing, material is taken off from rod, place on the vulcanizing press, in 150 ℃, compression moulding under the 10Mpa.Material is taken out, make the sample of desired shape, to be measured.
After measured, its resistivity is 44 Ω cm, and the smoke density value is 145, and oxygen index is 30.1.
Claims (10)
1. a conduction antiflaming ethylene-vinyl acetate composite material with low smoke is to be matrix with the ethylene-vinyl acetate, is filler with graphitized carbon black and palygorskite clay, by the macromole melt intercalated method, uniform filling is dispersed in the ethylene-vinyl acetate matrix.
2. conduct electricity antiflaming ethylene-vinyl acetate composite material with low smoke according to claim 1, it is characterized in that: the mass ratio of described ethylene-vinyl acetate and filler is 1: 0.1～1: 0.5.
3. conduct electricity antiflaming ethylene-vinyl acetate composite material with low smoke according to claim 1, it is characterized in that: in the described filler, the mass ratio of graphitized carbon black and polygorskite is 1: 1～1: 0.1.
4. conduct electricity the preparation method of antiflaming ethylene-vinyl acetate composite material with low smoke according to claim 1, be with the ethylene-vinyl acetate particle in 40～70 ℃ of following vacuum-drying 24～48h, place on the two roll plastic mixing mill heating and melting to flowing; The graphitized carbon black and the polygorskite filler that add 0.1～0.5 times of ethylene-vinyl acetate granular mass, in 110～150 ℃ mixing 0.1～0.4 hour, place then on the vulcanizing press, in 110～150 ℃, compression moulding under 8～10Mpa.
5. conduct electricity the preparation method of antiflaming ethylene-vinyl acetate composite material with low smoke according to claim 1, it is characterized in that: in the described filler, the mass ratio of graphitized carbon black and palygorskite clay is 1: 1～1: 0.1.
6. conduct electricity the preparation method of antiflaming ethylene-vinyl acetate composite material with low smoke according to claim 1, it is characterized in that: when adding filler, add ethylene-vinyl acetate granular mass 3.0 * 10
-3～5 * 10
-3Antioxidant doubly.
7. conduct electricity the preparation method of antiflaming ethylene-vinyl acetate composite material with low smoke according to claim 1, it is characterized in that: when adding filler, add the lubricant of 0.01～0.03 times of ethylene-vinyl acetate granular mass.
8. as the preparation method of conduction antiflaming ethylene-vinyl acetate composite material with low smoke as described in the claim 6, it is characterized in that: described antioxidant is 2,2-methylene-bis (4-methyl-6-tert butyl phenol), (3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid pentaerythritol ester or triphenyl phosphite.
9. as the preparation method of conduction antiflaming ethylene-vinyl acetate composite material with low smoke as described in the claim 7, it is characterized in that: described lubricant is two hard esteramides, glyceryl monostearate or Tristearoylglycerols of ethylene group.
10. have the preparation method of the ethylene-vinyl acetate composite material of conduction flame retardant properties according to claim 1, it is characterized in that: described graphitized carbon black is acetylene carbon black, paint, printing ink ordinary carbon black or superconduction carbon black.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102492214A (en) * | 2011-12-21 | 2012-06-13 | 西北师范大学 | Ethylene-vinyl acetate-based halogen-free flame retardant conductive high molecular composite material |
| CN103077765A (en) * | 2013-02-01 | 2013-05-01 | 南京信息工程大学 | Composite conducting material and preparation method thereof |
| CN111944231A (en) * | 2020-08-24 | 2020-11-17 | 安徽省康利亚股份有限公司 | Low-smoke halogen-free flame-retardant super-flexible oil-resistant cable material |
| CN116640377A (en) * | 2023-05-31 | 2023-08-25 | 江阴市海江高分子材料有限公司 | High-flame-retardance conductive material for automotive wires and cables and preparation method thereof |
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| CN101392079A (en) * | 2008-10-10 | 2009-03-25 | 常州天晟新材料股份有限公司 | Conductive ethylene-vinyl acetate co-polymer foamed profile and preparation method thereof |
| CN101544790A (en) * | 2009-04-17 | 2009-09-30 | 安徽纵横高科电缆股份有限公司 | 125 DEG C resistance low smoke non-halogen rubber-sheathed cable shielding material |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102492214A (en) * | 2011-12-21 | 2012-06-13 | 西北师范大学 | Ethylene-vinyl acetate-based halogen-free flame retardant conductive high molecular composite material |
| CN102492214B (en) * | 2011-12-21 | 2013-06-12 | 西北师范大学 | Ethylene-vinyl acetate-based halogen-free flame retardant conductive high molecular composite material |
| CN103077765A (en) * | 2013-02-01 | 2013-05-01 | 南京信息工程大学 | Composite conducting material and preparation method thereof |
| CN111944231A (en) * | 2020-08-24 | 2020-11-17 | 安徽省康利亚股份有限公司 | Low-smoke halogen-free flame-retardant super-flexible oil-resistant cable material |
| CN111944231B (en) * | 2020-08-24 | 2024-04-12 | 安徽省康利亚股份有限公司 | Low-smoke halogen-free flame-retardant super-flexible oil-resistant cable material |
| CN116640377A (en) * | 2023-05-31 | 2023-08-25 | 江阴市海江高分子材料有限公司 | High-flame-retardance conductive material for automotive wires and cables and preparation method thereof |
| CN116640377B (en) * | 2023-05-31 | 2024-04-02 | 江阴市海江高分子材料有限公司 | High-flame-retardance conductive material for automotive wires and cables and preparation method thereof |
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