CN102492214A - Ethylene-vinyl acetate-based halogen-free flame retardant conductive high molecular composite material - Google Patents
Ethylene-vinyl acetate-based halogen-free flame retardant conductive high molecular composite material Download PDFInfo
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Abstract
The invention provides a halogen-free flame retardant conductive high molecular composite material taking an ethylene-vinyl acetate copolymer as a substrate. The composite material is prepared by taking the ethylene-vinyl acetate copolymer as a substrate and taking paligorskite, triazine triamine phosphate, vermiculite and conductive carbon black as a composite adding system by means of fusing and internally mixing. As proved by tests, the oxygen index of the halogen-free flame retardant conductive composite material is 28.5-33.2, the horizontal combustion reaches a grade FH-1, and vertical combustion reaches a grade UL94V-0; electric resistivity is 104-100 ohm.cm, tensile strength is 10.7-12.2 MPa, elongation at break is 690.7-535.3 percent, smoke density (under a smoke-free condition) is 241-291, and various indexes fully meet the requirements of an industrial standard YD/T1113-2001; and the composite material is mainly used in the fields of building materials, electric wires, cables, electrical appliance manufacturing, electronic industry, and the like.
Description
Technical field
The invention belongs to the polymer composite field; Relate to a kind of polymer composite with fire-retardant and conducting function; Relating in particular to a kind of is the halogen-free flame-retardant conductive polymer composite of matrix with the ethylene-vinyl acetate copolymer, is mainly used in fields such as building materials, electric wire, household electrical appliances manufacturing and electron trade.
Background technology
Modification to polymkeric substance has become one of focus of present research and development, but along with The development in society and economy and progress, the polymer composite of simple function has not satisfied the demand of current people's lives.As everyone knows; These macromolecular material oxygen indexs of plastics, rubber, fiber and coating are very low; These material combustions in air, burn when being easy to meet naked light, in case will bring inestimable disaster and loss to the country and people's security of the lives and property; So fire retardant material is in building, very important effect is being brought into play in fields such as household electrical appliances.Because the Halogen fire retardant material be in case burning can discharge poisonous and corrosive gases, thereby its application receives strict restriction, so the agent of Halogen smoke-inhibiting flame retardant is arisen at the historic moment.In addition, the volume specific resistance of commodity polymer polymkeric substance is higher, hardly conduction; But plastics can produce static in production, transportation, use, product is prone to dust suction, is difficult for forming process; Also possibly cause burning and blast because of plastic static; And conducting polymer composite is widely used at numerous areas such as electric wire envelope curve, electronic industries, and it is significant therefore to develop the functional properties conductivity macromolecular material, and product also has boundless application prospect.
Chinese patent 200710134374.2 discloses a kind of with sheeted nanometer magnesium hydroxide, red phosphorus, expanded graphite; Trimeric cyanamide; Ammonium polyphosphate, tetramethylolmethane are the anti-flaming dope of composite flame-retardant agent preparation; Used chemotype expandable flame retardant system in this patent, but this system has easy moisture absorption, separates out, the shortcoming of poor heat stability; It is polymer-modified conduction fire-retardant filler with expanded graphite, red phosphorus, ammonium polyphosphate and triethyl phosphate that Chinese patent 200510095426.0 discloses a kind of; Though give polymkeric substance so certain conduction flame retardant properties is arranged; But because the less expanded graphite of density exists; Bring operation inconvenience, and the resistivity of prepared matrix material is higher, can not satisfy the requirement of most of industry.
Summary of the invention
The objective of the invention is provides a kind of halogen-free flame-retardant conductive polymer composite to the problem that exists in the prior art.
Halogen-free flame-retardant conductive polymer composite of the present invention is to be matrix with the ethylene-vinyl acetate copolymer, and with polygorskite, trimeric cyanamide polyphosphate, vermiculite, graphitized carbon black are moulded technology fusion banburying with the refining of routine and formed as compound interpolation system.
The polygorskite microstructure presents basic structural unit rod brilliant (excellent crystalline substance is needle-like) or the unit brilliant close parallel of rod is assembled the excellent druse that forms; They have the micropore consistent with length direction, and the hole contains ignition-proof element magnesium, aluminium, silicate and dissimilar water (crystal water, hydroxyl structure water, zeolite molecules water and inclusion water).In receiving thermal process, these water can be taken away heat and diluent air, and the contained MOX of polygorskite can be fine and close in addition covers the combustionmaterial surface, makes that the formed carbon-coating of other fire retardants is tightr.
The trimeric cyanamide polyphosphate can at high temperature produce the compound of phosphoric acid or phosphoric acid; The catalytic polymer matrix is cross-linked into charcoal; The charcoal layer that generates covers composite material surface, and this compound at high temperature also can produce a large amount of ammonias, the concentration of dilution inflammable gas and combustion-supporting gas.
In the matrix material combustion processes, vermiculite is with 200 ~ 300 times volumetric expansion, and the carbon-coating that makes polymkeric substance generate is tightr, thereby makes the heat-proof quality of carbon-coating improve greatly, plays the effect of cooperative flame retardant.
The optimum filling amount of graphitized carbon black in whole system makes it to reach percolation threshold, forms effective conductive network.
In this compound interpolation system, trimeric cyanamide polyphosphate and vermiculite are expansion type flame retardant, in matrix material fire-retardant, bear the effect of source of the gas, acid source and carbon source; Palygorskite clay plays the effect of fire retarding synergist through the concentration that discharges water vapor and reduce the combustionmaterial surface temperature and dilute flammable or combustion-supporting gas, and the MOX of its generation makes that the charcoal layer is tightr in addition; Graphitized carbon black had both been born the effect of conduction, also for polymer combustion forms solid carbon-coating a large amount of carbon resources was provided.
Affect the mechanical properties under the situation with machining property taking all factors into consideration flame retardant properties and electrical property and less, make composite flame-retardant agent and conductive filler material that the addition trim point an of the best arranged.A large amount of experiment proofs; When the addition of polygorskite is 5 ~ 20% of a matrix ethylene-vinyl acetate copolymer quality; The addition of trimeric cyanamide polyphosphate is 10 ~ 25% of a substrate quality; The addition of vermiculite is 3 ~ 15% of a substrate quality, and the addition of graphitized carbon black is controlled at 5 of substrate quality ~ 25% o'clock, and this matrix material all has good flame retardancy, electrical property and mechanical property.
Through measuring, the oxygen index of halogen-free flame-retardant conductive matrix material of the present invention is 28.5 ~ 33.2, and horizontal firing reaches the FH-1 level, and vertical combustion reaches the UL94V-0 level; Resistivity is 10
4Ω cm ~ 10
0Ω cm; Tensile strength is 10.7MPa ~ 12.2 MPa; Elongation at break is 690.7 ~ 535.3 %; Smoke density is (under the smokeless condition) 241 ~ 291, and all kinds of indexs satisfy the requirement of industry standard YD/T 1113-2001 fully, are mainly used in fields such as building materials, electric wire, household electrical appliances manufacturing and electron trade.
Embodiment
Be described further through the preparation and the performance of specific embodiment below matrix material of the present invention.
Embodiment 1: ethylene-vinyl acetate is placed Banbury mixer for 100 parts, at 120 ℃ of preheating 5min, add 0.25 part of inhibitor; 1.5 parts of lubricants; 5 parts of polygorskites, 10 parts of trimeric cyanamide polyphosphates, 3 parts of vermiculites; 5 parts of graphitized carbon black T-80, melt blending 15 min under 120 ℃ of conditions with rotating speed 60 rpm; Melt blended material is taken off behind compressing tablet on the vulcanizing press (120 ℃ of vulcanizing press temperature), place mould, preheating 5 min, hot pressing 7 min under 15 Mpa conditions, the 5 min moulding of under 15 Mpa, colding pressing rapidly then.Sample preparation on the RH-7010 sheet-punching machine.The sample of test oxygen index is 15 * 5 * 3 mm, and test resistance rate sample is 110 * 50 mm, and the test tensile property is the sample of dumbbell shaped.
Before the preparation, dry polymeric matrix and all fillers and auxiliary agent be dry 12 h under 70 ℃ all.
Test result is: oxygen index is 28.5, and horizontal firing reaches the FH-1 level, and vertical combustion reaches the UL94V-0 level; Resistivity is 10
4Ω cm, tensile strength is 12.2MPa, and elongation at break is 690.7 %, and smoke density is (under the smokeless condition) 291.
Embodiment 2: ethylene-vinyl acetate is placed Banbury mixer for 100 parts, at 130 ℃ of preheating 5min, add 0.25 part of inhibitor; 1.5 parts of lubricants; 20 parts of polygorskites, 25 parts of trimeric cyanamide polyphosphates, 25 parts of vermiculites; 25 parts of graphitized carbon black T-80, melt blending 15 min under 130 ℃ of conditions with rotating speed 60 rpm; Melt blended material is taken off behind compressing tablet on the vulcanizing press (130 ℃ of vulcanizing press temperature), place mould, preheating 5 min, hot pressing 7 min under 15 Mpa conditions, the 5 min moulding of under 15 Mpa, colding pressing rapidly then.Sample preparation on the RH-7010 sheet-punching machine.The sample of test oxygen index is 15 * 5 * 3 mm, and test resistance rate sample is 110 * 50 mm, and the test tensile property is the sample of dumbbell shaped.
Before the preparation, dry polymeric matrix and all fillers and auxiliary agent be dry 12 h under 70 ℃ all.
Test result is: oxygen index is 33.2, and horizontal firing reaches the FH-1 level, and vertical combustion reaches the UL94V-0 level; Resistivity is 10
0Ω cm, tensile strength is 10.7 MPa, and elongation at break is 535.3 %, and smoke density is (under the smokeless condition) 241.
Embodiment 3: ethylene-vinyl acetate is placed Banbury mixer for 100 parts, at 130 ℃ of preheating 5min, add 0.25 part of inhibitor; 1.5 parts of lubricants; 10 parts of polygorskites, 15 parts of trimeric cyanamide polyphosphates, 7 parts of vermiculites; 15 parts of graphitized carbon black VXC-72R, melt blending 15 min under 130 ℃ of conditions with rotating speed 60 rpm; Melt blended material is taken off behind compressing tablet on the vulcanizing press (130 ℃ of vulcanizing press temperature), place mould, preheating 5 min, hot pressing 7 min under 15 Mpa conditions, the 5 min moulding of under 15 Mpa, colding pressing rapidly then.Sample preparation on the RH-7010 sheet-punching machine.The sample of test oxygen index is 15 * 5 * 3 mm, and test resistance rate sample is 110 * 50 mm, and the test tensile property is the sample of dumbbell shaped.
Before the preparation, dry polymeric matrix and all fillers and auxiliary agent be dry 12 h under 70 ℃ all.
Test result is: oxygen index is 30, and horizontal firing reaches the FH-1 level, and vertical combustion reaches the UL94V-0 level; Resistivity is 320 Ω cm, and tensile strength is 10.9 MPa, and elongation at break is 668.6 %, and smoke density is (under the smokeless condition) 262.
Embodiment 4: ethylene-vinyl acetate is placed Banbury mixer for 100 parts, at 130 ℃ of preheating 5min, add 0.25 part of inhibitor; 1.5 parts of lubricants; 15 parts of polygorskites, 10 parts of trimeric cyanamide polyphosphates, 9 parts of vermiculites; 20 parts of graphitized carbon black F-900, melt blending 15 min under 130 ℃ of conditions with rotating speed 60 rpm; Melt blended material is taken off behind compressing tablet on the vulcanizing press (130 ℃ of vulcanizing press temperature), place mould, preheating 5 min, hot pressing 7 min under 15 Mpa conditions, the 5 min moulding of under 15 Mpa, colding pressing rapidly then.Sample preparation on the RH-7010 sheet-punching machine.The sample of test oxygen index is 15 * 5 * 3 mm, and test resistance rate sample is 110 * 50 mm, and the test tensile property is the sample of dumbbell shaped.
Before the preparation, dry polymeric matrix and all fillers and auxiliary agent be dry 12 h under 70 ℃ all.
Test result is: oxygen index is 29.0, and horizontal firing reaches the FH-1 level, and vertical combustion reaches the UL94V-0 level; Resistivity is 72.6 Ω cm, and tensile strength is 11.8 MPa, and elongation at break is 675.3 %, and smoke density is (under the smokeless condition) 270.
Embodiment 5: ethylene-vinyl acetate is placed Banbury mixer for 100 parts, at 130 ℃ of preheating 5min, add 0.25 part of inhibitor; 1.5 parts of lubricants; 10 parts of polygorskites, 20 parts of trimeric cyanamide polyphosphates, 10 parts of vermiculites; 15 parts of graphitized carbon black F-900, melt blending 15 min under 130 ℃ of conditions with rotating speed 60 rpm; Melt blended material is taken off behind compressing tablet on the vulcanizing press (130 ℃ of vulcanizing press temperature), place mould, preheating 5 min, hot pressing 7 min under 15 Mpa conditions, the 5 min moulding of under 15 Mpa, colding pressing rapidly then.Sample preparation on the RH-7010 sheet-punching machine.The sample of test oxygen index is 15 * 5 * 3 mm, and test resistance rate sample is 110 * 50 mm, and the test tensile property is the sample of dumbbell shaped.
Before the preparation, dry polymeric matrix and all fillers and auxiliary agent be dry 12 h under 70 ℃ all.
Test result is: oxygen index is 33.1, and horizontal firing reaches the FH-1 level, and vertical combustion reaches the UL94V-0 level; Resistivity is 290 Ω cm, and tensile strength is 11.5 MPa, and elongation at break is 589.2 %, and smoke density is (under the smokeless condition) 269.
Embodiment 6: ethylene-vinyl acetate is placed Banbury mixer for 100 parts, at 130 ℃ of preheating 5min, add 0.25 part of inhibitor; 1.5 parts of lubricants; 10 parts of polygorskites, 10 parts of trimeric cyanamide polyphosphates, 15 parts of vermiculites; 20 parts of graphitized carbon black T-80, melt blending 15 min under 130 ℃ of conditions with rotating speed 60 rpm; Melt blended material is taken off behind compressing tablet on the vulcanizing press (130 ℃ of vulcanizing press temperature), place mould, preheating 5 min, hot pressing 7 min under 15 Mpa conditions, the 5 min moulding of under 15 Mpa, colding pressing rapidly then.Sample preparation on the RH-7010 sheet-punching machine.The sample of test oxygen index is 15 * 5 * 3 mm, and test resistance rate sample is 110 * 50 mm, and the test tensile property is the sample of dumbbell shaped.
Before the preparation, dry polymeric matrix and all fillers and auxiliary agent be dry 12 h under 70 ℃ all.
Test result is: oxygen index is 32.8, and horizontal firing reaches the FH-1 level, and vertical combustion reaches the UL94V-0 level; Resistivity is 65.9 Ω cm, and tensile strength is 11.0 MPa, and elongation at break is 670.3%, and smoke density is (under the smokeless condition) 251.
Embodiment 7: ethylene-vinyl acetate is placed Banbury mixer for 100 parts, at 130 ℃ of preheating 5min, add 0.25 part of inhibitor; 1.5 parts of lubricants; 9 parts of polygorskites, 23 parts of trimeric cyanamide polyphosphates, 11 parts of vermiculites; 15 parts of graphitized carbon black VXC-72R, melt blending 15 min under 130 ℃ of conditions with rotating speed 60 rpm; Melt blended material is taken off behind compressing tablet on the vulcanizing press (130 ℃ of vulcanizing press temperature), place mould, preheating 5 min, hot pressing 7 min under 15 Mpa conditions, the 5 min moulding of under 15 Mpa, colding pressing rapidly then.Sample preparation on the RH-7010 sheet-punching machine.The sample of test oxygen index is 15 * 5 * 3 mm, and test resistance rate sample is 110 * 50 mm, and the test tensile property is the sample of dumbbell shaped.
Before the preparation, dry polymeric matrix and all fillers and auxiliary agent be dry 12 h under 70 ℃ all.
Test result is: oxygen index is 30.2, and horizontal firing reaches the FH-1 level, and vertical combustion reaches the UL94V-0 level; Resistivity is 210 Ω cm, and tensile strength is 11.5 MPa, and elongation at break is 620.4 %, and smoke density is (under the smokeless condition) 260.
Among above-mentioned each embodiment; Inhibitor, lubricant all adopt conventional inhibitor (like triphenyl phosphite, (3, the 5-di-tert-butyl-hydroxy phenyl) propionic acid pentaerythritol ester; 2; 2-methylene-bis (4-methyl-6-tert butyl phenol)), lubricant (like second glyceryl monostearate (GMS), Tristearoylglycerol (HTG), the two hard esteramides (EBS) of support base).
Claims (6)
1. ethylene-vinyl acetate base halogen-free flame-retardant conductive polymer composite; Be to be matrix with the ethylene-vinyl acetate copolymer; With polygorskite, trimeric cyanamide polyphosphate, vermiculite, graphitized carbon black are compound interpolation system, mould technology fusion banburying with the refining of routine and form.
2. ethylene-vinyl acetate base halogen-free flame-retardant conductive polymer composite according to claim 1, it is characterized in that: the addition of said polygorskite is 5 ~ 20% of a matrix ethylene-vinyl acetate copolymer quality.
3. ethylene-vinyl acetate base halogen-free flame-retardant conductive polymer composite according to claim 1, it is characterized in that: the addition of said trimeric cyanamide polyphosphate is 10 ~ 25% of a matrix ethylene-vinyl acetate copolymer quality.
4. ethylene-vinyl acetate base halogen-free flame-retardant conductive polymer composite according to claim 1, it is characterized in that: the addition of said vermiculite is 3 ~ 15% of a matrix ethylene-vinyl acetate copolymer quality.
5. ethylene-vinyl acetate base halogen-free flame-retardant conductive polymer composite according to claim 1, it is characterized in that: the addition of said graphitized carbon black is 5 ~ 25% of a matrix ethylene-vinyl acetate copolymer quality.
6. ethylene-vinyl acetate base halogen-free flame-retardant conductive polymer composite according to claim 1, it is characterized in that: said graphitized carbon black is F-900, T-80, VXC-72R.
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| CN113354874A (en) * | 2021-06-10 | 2021-09-07 | 湖北工程学院 | Preparation method of composite additive, wood-plastic board and preparation method thereof |
| CN114672091A (en) * | 2022-02-22 | 2022-06-28 | 浙江师范大学 | Method for simultaneously improving multiple properties of ethylene-vinyl acetate copolymer |
| 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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| 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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