CN103951846A - Application of carbon nanotube as composition flame retardation anti-dripping agent - Google Patents
Application of carbon nanotube as composition flame retardation anti-dripping agent Download PDFInfo
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Abstract
The invention provides an application of a carbon nanotube as a composition flame retardation anti-dripping agent, the carbon nanotube comprises the carbon nanotube with unmodified surface or the carbon nanotube with hydroxylated surface or the carbon nanotube with carboxylated surface, carbon nanotube is added in the flame retardation material for being as the anti-dripping agent so as to replace a traditional polytetrafluoroethylene anti-dripping agent, under the condition that the addition amount is same, the effect of the composition flame retardation anti-dripping agent is better than that of the polytetrafluoroethylene anti-dripping agent.
Description
Technical field
The present invention relates to the flame-retardant modified field of macromolecular material, relate in particular to the purposes of a kind of carbon nanotube as the agent of composition flame-retardant anti-dropping.
Background technology
Along with the development of modern science and technology, people are also more and more stricter to the fire-retardant requirement of polymkeric substance.Many times all require common plastics (as: material such as polyethylene, polypropylene, polymeric amide, polycarbonate, acrylonitrile-butadiene-styrene resin, polyester) can reach good flame retardant effect, i.e. the V0 rank of UL-94 or higher 5V rank.
With regard to current flame retardance of polymer, mainly contain that Halogen is fire-retardant, the large class of halogen-free flameproof two.In practical study and application, also to reach desirable flame retardant effect no matter be the fire-retardant or halogen-free flameproof of Halogen for the consumption that reduces main flame retardant, often in polymkeric substance, add the composite use of anti-dripping agent and main flame retardant, can play so good flame retardant effect.Anti-dripping agent is almost PTFE Type anti-dripping agent on the market entirely at present.
For now, carbon nanotube is mainly used for that preparation strengthens, toughness reinforcing plastic base composite material, heat conduction, conduction, anlistatig plastic base composite material, and be mixed with metal-base composites etc. with metal powder and metallic compound (or nonmetallic compound).For example: Chinese patent CN 103173000 A, are used for enhancing, toughened polymer phenylate and nylon composite materials by carbon nanotube; Chinese patent CN 100569851 C, are used for enhancing, epoxy resin toughened by carbon nanotube; Chinese patent CN 100487046 C, are mainly used in tenacity-increased profax by carbon nanotube; Chinese patent CN 102418164 A, for polysulfonamides, have prepared Antistatic polysulfonamide/carbon nano-tube composite material by carbon nanotube; Chinese patent CN 102583315 A, are mixed with matrix material by carbon nanotube and Z 250; Chinese patent CN 102002652 B, are mixed with matrix material by carbon nanotube and metal powder.So the present invention uses carbon nanotube as anti-dripping agent, and its effect is compared with traditional anti-dripping agent (tetrafluoroethylene), and the in the situation that of same amount, its effect is better than traditional anti-dripping agent.
Summary of the invention
The object of the present invention is to provide the purposes of a kind of carbon nanotube as the agent of composition flame-retardant anti-dropping, the present invention proposes first carbon nanotube and uses as the agent of composition flame-retardant anti-dropping, alternative traditional anti-dripping agent, and anti-drippage effect is remarkable.
A kind of carbon nanotube of the present invention is as the purposes of composition flame-retardant anti-dropping agent, and described carbon nanotube is that surface does not have the carbon nanotube of modification or for the carbon nanotube of surface hydroxylation or be the carboxylated carbon nanotube in surface.
Described carbon nanotube can be Single Walled Carbon Nanotube, and its external diameter 1 ~ 2 nanometer, length are at 5 ~ 30 microns, purity > 90wt%.
Described carbon nanotube can be multi-walled carbon nano-tubes, and its external diameter < 8 nanometers, length are at 10 ~ 30 microns, purity > 98wt%.
Described carbon nanotube can be double-walled carbon nano-tube, and its external diameter 2 ~ 4 nanometers, length are at 5 ~ 15 microns, purity > 60wt%.
The hydroxy radical content of the carbon nanotube of described surface hydroxylation is good at 3.8wt% ~ 5.8wt%.
The carboxyl-content of the carboxylated carbon nanotube in described surface is good at 2.7wt% ~ 3.9wt%.
In the present invention, the body material in described composition is polyethylene, polypropylene, polymeric amide, polycarbonate, acrylonitrile-butadiene-styrene resin, polyethylene terephthalate or polybutylene terephthalate.Wherein, polymeric amide is one or more in polyamide 6, polyamide 66, polyamide 610, polymeric amide 46, polyamide 1010, polyamide 612, polymeric amide 12, polymeric amide 8, polymeric amide 9.
In described composition, the consumption of carbon nanotube is the 0.1%-1% of composition substrate quality of materials.
In described composition, taking composition substrate quality of materials as benchmark, also include 12wt% ~ 30wt% fire retardant, 0.2wt% ~ 0.5wt% oxidation inhibitor, 0.1wt% ~ 0.3wt% lubricant and the steady agent of 0.1wt% ~ 0.3wt% light, in the time preparing composition material, can add fire retardant, oxidation inhibitor, lubricant, the steady agent of light to carry out extruding pelletization simultaneously.
Above-mentioned fire retardant is selected one or more of TDE, brominated epoxy resin, tetrabromo-bisphenol, chlorinatedpolyethylene, antimonous oxide, Halogen nitrogen phosphorus fire retardant.
Above-mentioned oxidation inhibitor is selected four [β-(3; 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester (antioxidant 1010), three [2; 4-di-tert-butyl-phenyl] phosphorous acid ester (irgasfos 168), N; N'-pair-(3-(3; 5-di-tert-butyl-hydroxy phenyl) propionyl) in hexanediamine (oxidation inhibitor 1098), β-(3,5-di-tert-butyl-hydroxy phenyl) positive octadecanol ester of propionic acid (antioxidant 1076) two kinds carry out composite use.
Above-mentioned lubricant is ethylene bis stearamide (EBS).
The steady agent of above-mentioned light is 50% hindered amine as light stabilizer 2,2,6,6-tetramethyl--4-low polypropylene miser of piperidine alcohols stearate (UV-3853PP5) and 2-(2-hydroxyl-uncle 5-good fortune base phenyl) benzotriazole (UV-5411) carries out the composite use of 1:1.
Beneficial effect of the present invention is:
1. the present invention is using carbon nanotube as anti-dripping agent, with traditional anti-dripping agent---and compared with PTFE Type anti-dripping agent, anti-drippage effect significantly improves.
2. traditional carbon nanotube is mainly used for that preparation strengthens, toughness reinforcing plastic base composite material, heat conduction, conduction, anlistatig plastic base composite material, and be mixed with metal-base composites etc. with metal powder and metallic compound (or nonmetallic compound); And the present invention sets it as anti-dripping agent use, the 0.1wt%-1wt% that its consumption is matrix resin.
3. widen the use range of carbon nanotube, broken the unicity of market anti-dripping agent.
Embodiment
Below in conjunction with some embodiment and comparative example, the invention will be further described.
The material of using in embodiment and comparative example has:
Single Walled Carbon Nanotube A model: CNT200(contains hydroxyl in surface, hydroxy radical content 3.96wt%) Beijing Deco Dao Jin Science and Technology Ltd.;
Single Walled Carbon Nanotube B model: CNT300(contains carboxyl in surface, carboxyl-content 2.73wt%) Beijing Deco Dao Jin Science and Technology Ltd.;
Multi-walled carbon nano-tubes A model: CNT202(contains hydroxyl in surface, hydroxy radical content 5.58wt%) Beijing Deco Dao Jin Science and Technology Ltd.;
Multi-walled carbon nano-tubes B model: CNT302(contains carboxyl in surface, carboxyl-content 3.86wt%) Beijing Deco Dao Jin Science and Technology Ltd.;
Double-walled carbon nano-tube A model: CNT210(contains hydroxyl in surface, hydroxy radical content 3.96wt%) Beijing Deco Dao Jin Science and Technology Ltd.;
Double-walled carbon nano-tube B model: CNT310(contains carboxyl in surface, carboxyl-content 2.73wt%) Beijing Deco Dao Jin Science and Technology Ltd.;
Polypropylene model: PP BX3800 Korea S SK;
Polycarbonate model: PC 7022IR Mitsubishi;
Acrylonitrile-butadiene-styrene resin model: Dagu, ABS DG417 Tianjin chemical industry;
Polymeric amide model: PA6 M2500 newly understands in Guangzhou U.S.A and reaches;
Polyethylene terephthalate model: PET CB-608S far spins industry (Shanghai);
Fire retardant A model: sky, TDE Shandong one chemistry;
Fire retardant B model: sky, brominated epoxy resin Shandong one chemistry;
Fire retardant C model: sky, tetrabromo-bisphenol Shandong one chemistry;
Fire retardant D model: chlorinatedpolyethylene 2135 Weifang AsiaSat chemistry;
Fire retardant E model: antimonous oxide Yiyang stibium trioxide factory of Hengchang;
Fire retardant F model: Halogen nitrogen phosphorus fire retardant WR03 Suzhou peace letter is safe;
Anti-dripping agent model: the celestial nation in PTFE PTF-5050 Shanghai chemistry;
Oxidation inhibitor A model: Irganox1010 Switzerland Ciba;
Oxidation inhibitor B model: Irganox1098 Switzerland Ciba;
Oxidation inhibitor C model: Irganox1076 Switzerland Ciba;
Oxidation inhibitor D model: Irganox168 Switzerland Ciba;
Lubricant model: Chaoyang Chemical Co., Ltd. of EBS Indonesia;
The steady agent A of light model: UV-3853PP5 U.S. cyanogen spy;
The steady agent B of light model: UV-5411 U.S. cyanogen spy.
Following flame retardant test project, carries out UL-94 standard.
The listed embodiment of the present invention is exemplary embodiments of the present invention, and so protection scope of the present invention is not limited to this.
embodiment 1
Be the polypropylene PP BX3800 of 100 parts by weight part, the fire retardant A(TDE of 21 parts), the fire retardant E(antimonous oxide of 7 parts), 0.1 part of Single Walled Carbon Nanotube B, 0.1 part of oxidation inhibitor A, 0.1 part of oxidation inhibitor D, 0.1 part of Lubricate EBS, 0.05 part of steady agent A of light, 0.05 part of steady agent B of light add in high-speed mixer and mix.Wherein, the temperature of high-speed mixer is that 65 DEG C, the speed of high-speed mixer are 100 revs/min.Then the material mixing is added in twin screw extruder extrude, cooling, granulation, dress bag.The temperature of forcing machine is followed successively by 180 DEG C, 205 DEG C, 205 DEG C, 200 DEG C, 200 DEG C, 200 DEG C, 195 DEG C, 195 DEG C from feeding section to head, screw speed is 180 revs/min, and screw slenderness ratio is 40.Its flame retardant properties is in Table-1.
comparative example 1
Be the polypropylene PP BX3800 of 100 parts by weight part, the fire retardant A(TDE of 21 parts), the fire retardant E(antimonous oxide of 7 parts), 0.1 part of oxidation inhibitor A, 0.1 part of oxidation inhibitor D, 0.1 part of Lubricate EBS, 0.05 part of steady agent A of light, 0.05 part of steady agent B of light add in high-speed mixer and mix.Wherein, the temperature of high-speed mixer is that 65 DEG C, the speed of high-speed mixer are 100 revs/min.Then the material mixing is added in twin screw extruder extrude, cooling, granulation, dress bag.The temperature of forcing machine is followed successively by 180 DEG C, 205 DEG C, 205 DEG C, 200 DEG C, 200 DEG C, 200 DEG C, 195 DEG C, 195 DEG C from feeding section to head, screw speed is 180 revs/min, and screw slenderness ratio is 40.Its flame retardant properties is in Table-1.
embodiment 2
Be the polypropylene PP BX3800 of 100 parts by weight part, the fire retardant F of 30 parts, 0.5 part of Single Walled Carbon Nanotube A, 0.25 part of oxidation inhibitor A, 0.25 part of oxidation inhibitor D, 0.3 part of Lubricate EBS, 0.15 part of steady agent A of light, 0.15 part of steady agent B of light add in high-speed mixer and mix.Wherein, the temperature of high-speed mixer is that 75 DEG C, the speed of high-speed mixer are 120 revs/min.Then the material mixing is added in twin screw extruder extrude, cooling, granulation, dress bag.The temperature of forcing machine is followed successively by 180 DEG C, 205 DEG C, 205 DEG C, 200 DEG C, 200 DEG C, 200 DEG C, 195 DEG C, 195 DEG C from feeding section to head, screw speed is 220 revs/min, and screw slenderness ratio is 44.Its flame retardant properties is in Table-1.
comparative example 2
Be the polypropylene PP BX3800 of 100 parts by weight part, the fire retardant F of 30 parts, 0.25 part of oxidation inhibitor A, 0.25 part of oxidation inhibitor D, 0.3 part of Lubricate EBS, 0.15 part of steady agent A of light, 0.15 part of steady agent B of light add in high-speed mixer and mix.Wherein, the temperature of high-speed mixer is that 75 DEG C, the speed of high-speed mixer are 120 revs/min.Then the material mixing is added in twin screw extruder extrude, cooling, granulation, dress bag.The temperature of forcing machine is followed successively by 180 DEG C, 205 DEG C, 205 DEG C, 200 DEG C, 200 DEG C, 200 DEG C, 195 DEG C, 195 DEG C from feeding section to head, screw speed is 220 revs/min, and screw slenderness ratio is 44.Its flame retardant properties is in Table-1.
embodiment 3
Be the polypropylene PP BX3800 of 100 parts by weight part, the fire retardant F of 28 parts, 1 part of Single Walled Carbon Nanotube A, 0.2 part of oxidation inhibitor A, 0.25 part of oxidation inhibitor D, 0.25 part of Lubricate EBS, 0.1 part of steady agent A of light, 0.1 part of steady agent B of light add in high-speed mixer and mix.Wherein, the temperature of high-speed mixer is that 70 DEG C, the speed of high-speed mixer are 120 revs/min.Then the material mixing is added in twin screw extruder extrude, cooling, granulation, dress bag.The temperature of forcing machine is followed successively by 180 DEG C, 205 DEG C, 205 DEG C, 200 DEG C, 200 DEG C, 200 DEG C, 195 DEG C, 195 DEG C from feeding section to head, screw speed is 220 revs/min, and screw slenderness ratio is 44.Its flame retardant properties is in Table-1.
comparative example 3
Be the polypropylene PP BX3800 of 100 parts by weight part, the fire retardant F of 28 parts, 0.2 part of oxidation inhibitor A, 0.25 part of oxidation inhibitor D, 0.25 part of Lubricate EBS, 0.1 part of steady agent A of light, 0.1 part of steady agent B of light add in high-speed mixer and mix.Wherein, the temperature of high-speed mixer is that 70 DEG C, the speed of high-speed mixer are 120 revs/min.Then the material mixing is added in twin screw extruder extrude, cooling, granulation, dress bag.The temperature of forcing machine is followed successively by 180 DEG C, 205 DEG C, 205 DEG C, 200 DEG C, 200 DEG C, 200 DEG C, 195 DEG C, 195 DEG C from feeding section to head, screw speed is 220 revs/min, and screw slenderness ratio is 44.Its flame retardant properties is in Table-1.
comparative example 4
Be the polypropylene PP BX3800 of 100 parts by weight part, the fire retardant F of 28 parts, 1 part of anti-dripping agent PTF-5050,0.2 part of oxidation inhibitor A, 0.25 part of oxidation inhibitor D, 0.25 part of Lubricate EBS, 0.1 part of steady agent A of light, 0.1 part of steady agent B of light add in high-speed mixer and mix.Wherein, the temperature of high-speed mixer is that 70 DEG C, the speed of high-speed mixer are 120 revs/min.Then the material mixing is added in twin screw extruder extrude, cooling, granulation, dress bag.The temperature of forcing machine is followed successively by 180 DEG C, 205 DEG C, 205 DEG C, 200 DEG C, 200 DEG C, 200 DEG C, 195 DEG C, 195 DEG C from feeding section to head, screw speed is 220 revs/min, and screw slenderness ratio is 44.Its flame retardant properties is in Table-1.
The flame retardant properties of table-1 embodiment 1-3 and comparative example 1 ~ 4
| Test event | Embodiment 1 | Comparative example 1 | Embodiment 2 | Comparative example 2 | Embodiment 3 | Comparative example 3 | Comparative example 4 |
| UL-94 flame retardant rating | V0 | V0 | V0 | V0 | V0 | V0 | V0 |
| The t1+t2 summation (second) of 5 battens | 10 | 20 | 8 | 15 | 12 | 21 | 15 |
From above embodiment 1 ~ 3 and comparative example 1 ~ 3, can obviously find out, add carbon nanotube of the present invention to use as anti-dripping agent effective more a lot of than not adding; Can obviously find out from embodiment 1 and comparative example 1, the t1+t2 summation that adds 5 samples of carbon nanotube is 10 seconds, and the t1+t2 summation that does not add 5 samples of carbon nanotube is 20 seconds.On the other hand, from embodiment 3, comparative example 3 and comparative example 4 relatively can find out, the in the situation that of same amount, anti-dripping agent of the present invention is more effective than traditional PTFE type anti-dripping agent.
embodiment 4
Be the polycarbonate 7022IR of 100 parts by weight part, the fire retardant C of 9 parts, the fire retardant E of 3 parts, the multi-walled carbon nano-tubes B of 0.3 part, 0.15 part of oxidation inhibitor C, 0.25 part of oxidation inhibitor D, 0.15 part of Lubricate EBS, 0.12 part of steady agent A of light, 0.12 part of steady agent B of light adds in high-speed mixer and mixes.Wherein, the temperature of high-speed mixer is that 70 DEG C, the speed of high-speed mixer are 120 revs/min.Then the material mixing is added in twin screw extruder extrude, cooling, granulation, dress bag.The temperature of forcing machine is followed successively by 230 DEG C, 275 DEG C, 275 DEG C, 270 DEG C, 270 DEG C, 270 DEG C, 265 DEG C, 265 DEG C from feeding section to head, screw speed is 220 revs/min, and screw slenderness ratio is 40.Its flame retardant properties is in Table-2.
comparative example 5
Be the polycarbonate 7022IR of 100 parts by weight part, the fire retardant C of 9 parts, the fire retardant E of 3 parts, 0.15 part of oxidation inhibitor C, 0.25 part of oxidation inhibitor D, 0.15 part of Lubricate EBS, 0.12 part of steady agent A of light, 0.12 part of steady agent B of light adds in high-speed mixer and mixes.Wherein, the temperature of high-speed mixer is that 70 DEG C, the speed of high-speed mixer are 120 revs/min.Then the material mixing is added in twin screw extruder extrude, cooling, granulation, dress bag.The temperature of forcing machine is followed successively by 230 DEG C, 275 DEG C, 275 DEG C, 270 DEG C, 270 DEG C, 270 DEG C, 265 DEG C, 265 DEG C from feeding section to head, screw speed is 220 revs/min, and screw slenderness ratio is 40.Its flame retardant properties is in Table-2.
embodiment 5
Be the polycarbonate 7022IR of 100 parts by weight part, the fire retardant C of 10 parts, the fire retardant E of 3.5 parts, the multi-walled carbon nano-tubes A of 0.8 part, 0.2 part of oxidation inhibitor C, 0.3 part of oxidation inhibitor D, 0.25 part of Lubricate EBS, 0.15 part of steady agent A of light, 0.15 part of steady agent B of light add in high-speed mixer and mix.Wherein, the temperature of high-speed mixer is that 70 DEG C, the speed of high-speed mixer are 120 revs/min.Then the material mixing is added in twin screw extruder extrude, cooling, granulation, dress bag.The temperature of forcing machine is followed successively by 230 DEG C, 275 DEG C, 275 DEG C, 270 DEG C, 270 DEG C, 270 DEG C, 265 DEG C, 265 DEG C from feeding section to head, screw speed is 220 revs/min, and screw slenderness ratio is 40.Its flame retardant properties is in Table-2.
comparative example 6
Be the polycarbonate 7022IR of 100 parts by weight part, the fire retardant C of 10 parts, the fire retardant E of 3.5 parts, 0.2 part of oxidation inhibitor C, 0.3 part of oxidation inhibitor D, 0.25 part of Lubricate EBS, 0.15 part of steady agent A of light, 0.15 part of steady agent B of light adds in high-speed mixer and mixes.Wherein, the temperature of high-speed mixer is that 70 DEG C, the speed of high-speed mixer are 120 revs/min.Then the material mixing is added in twin screw extruder extrude, cooling, granulation, dress bag.The temperature of forcing machine is followed successively by 230 DEG C, 275 DEG C, 275 DEG C, 270 DEG C, 270 DEG C, 270 DEG C, 265 DEG C, 265 DEG C from feeding section to head, screw speed is 220 revs/min, and screw slenderness ratio is 40.Its flame retardant properties is in Table-2.
embodiment 6
Be the polycarbonate 7022IR of 100 parts by weight part, the fire retardant C of 11 parts, the fire retardant E of 4 parts, the multi-walled carbon nano-tubes B of 1 part, 0.2 part of oxidation inhibitor C, 0.3 part of oxidation inhibitor D, 0.25 part of Lubricate EBS, 0.15 part of steady agent A of light, 0.15 part of steady agent B of light add in high-speed mixer and mix.Wherein, the temperature of high-speed mixer is that 70 DEG C, the speed of high-speed mixer are 120 revs/min.Then the material mixing is added in twin screw extruder extrude, cooling, granulation, dress bag.The temperature of forcing machine is followed successively by 230 DEG C, 275 DEG C, 275 DEG C, 270 DEG C, 270 DEG C, 270 DEG C, 265 DEG C, 265 DEG C from feeding section to head, screw speed is 220 revs/min, and screw slenderness ratio is 40.Its flame retardant properties is in Table-2.
comparative example 7
Be the polycarbonate 7022IR of 100 parts by weight part, the fire retardant C of 11 parts, the fire retardant E of 4 parts, 0.2 part of oxidation inhibitor C, 0.3 part of oxidation inhibitor D, 0.25 part of Lubricate EBS, 0.15 part of steady agent A of light, 0.15 part of steady agent B of light add in high-speed mixer and mix.Wherein, the temperature of high-speed mixer is that 70 DEG C, the speed of high-speed mixer are 120 revs/min.Then the material mixing is added in twin screw extruder extrude, cooling, granulation, dress bag.The temperature of forcing machine is followed successively by 230 DEG C, 275 DEG C, 275 DEG C, 270 DEG C, 270 DEG C, 270 DEG C, 265 DEG C, 265 DEG C from feeding section to head, screw speed is 220 revs/min, and screw slenderness ratio is 40.Its flame retardant properties is in Table-2.
comparative example 8
Be the polycarbonate 7022IR of 100 parts by weight part, the fire retardant C of 11 parts, the fire retardant E of 4 parts, the anti-dripping agent PTF-5050 of 1 part, 0.2 part of oxidation inhibitor C, 0.3 part of oxidation inhibitor D, 0.25 part of Lubricate EBS, 0.15 part of steady agent A of light, 0.15 part of steady agent B of light add in high-speed mixer and mix.Wherein, the temperature of high-speed mixer is that 70 DEG C, the speed of high-speed mixer are 120 revs/min.Then the material mixing is added in twin screw extruder extrude, cooling, granulation, dress bag.The temperature of forcing machine is followed successively by 230 DEG C, 275 DEG C, 275 DEG C, 270 DEG C, 270 DEG C, 270 DEG C, 265 DEG C, 265 DEG C from feeding section to head, screw speed is 220 revs/min, and screw slenderness ratio is 40.Its flame retardant properties is in Table-2.
The flame retardant properties of table-2 embodiment 4-6 and comparative example 5 ~ 8
| Test event | Embodiment 4 | Comparative example 5 | Embodiment 5 | Comparative example 6 | Embodiment 6 | Comparative example 7 | Comparative example 8 |
| UL-94 flame retardant rating | V0 | V0 | V0 | V0 | V0 | V0 | V0 |
| The t1+t2 summation (second) of 5 battens | 10 | 18 | 6 | 11 | 2 | 10 | 5 |
From above embodiment 4 ~ 6 and comparative example 5 ~ 7, can obviously find out, add carbon nanotube of the present invention to use as anti-dripping agent effective more a lot of than not adding; Can obviously find out from embodiment 6 and comparative example 7, the t1+t2 summation that adds 5 samples of carbon nanotube is 2 seconds, and the t1+t2 summation that does not add 5 samples of carbon nanotube is 10 seconds.On the other hand, from embodiment 6, comparative example 6 and comparative example 8 relatively can find out, the in the situation that of same amount, anti-dripping agent of the present invention is more effective than traditional PTFE type anti-dripping agent.
embodiment 7
Be the ABS DG417 of 100 parts by weight part, the fire retardant B of 15 parts, the fire retardant E of 5 parts, the fire retardant D of 8 parts, the double-walled carbon nano-tube B of 0.2 part, 0.2 part of oxidation inhibitor C, 0.3 part of oxidation inhibitor D, 0.25 part of Lubricate EBS, 0.15 part of steady agent A of light, 0.15 part of steady agent B of light add in high-speed mixer and mix.Wherein, the temperature of high-speed mixer is that 70 DEG C, the speed of high-speed mixer are 120 revs/min.Then the material mixing is added in twin screw extruder extrude, cooling, granulation, dress bag.The temperature of forcing machine is followed successively by 200 DEG C, 225 DEG C, 225 DEG C, 220 DEG C, 220 DEG C, 220 DEG C, 215 DEG C, 215 DEG C from feeding section to head, screw speed is 200 revs/min, and screw slenderness ratio is 44.Its flame retardant properties is in Table-3.
comparative example 9
Be the ABS DG417 of 100 parts by weight part, the fire retardant B of 15 parts, the fire retardant E of 5 parts, the fire retardant D of 8 parts, 0.2 part of oxidation inhibitor C, 0.3 part of oxidation inhibitor D, 0.25 part of Lubricate EBS, 0.15 part of steady agent A of light, 0.15 part of steady agent B of light add in high-speed mixer and mix.Wherein, the temperature of high-speed mixer is that 70 DEG C, the speed of high-speed mixer are 120 revs/min.Then the material mixing is added in twin screw extruder extrude, cooling, granulation, dress bag.The temperature of forcing machine is followed successively by 200 DEG C, 225 DEG C, 225 DEG C, 220 DEG C, 220 DEG C, 220 DEG C, 215 DEG C, 215 DEG C from feeding section to head, screw speed is 200 revs/min, and screw slenderness ratio is 44.Its flame retardant properties is in Table-3.
embodiment 8
Be the ABS DG417 of 100 parts by weight part, the fire retardant B of 13 parts, the fire retardant E of 5 parts, the fire retardant D of 5 parts, the double-walled carbon nano-tube A of 0.6 part, 0.2 part of oxidation inhibitor C, 0.3 part of oxidation inhibitor D, 0.25 part of Lubricate EBS, 0.15 part of steady agent A of light, 0.15 part of steady agent B of light add in high-speed mixer and mix.Wherein, the temperature of high-speed mixer is that 70 DEG C, the speed of high-speed mixer are 120 revs/min.Then the material mixing is added in twin screw extruder extrude, cooling, granulation, dress bag.The temperature of forcing machine is followed successively by 200 DEG C, 225 DEG C, 225 DEG C, 220 DEG C, 220 DEG C, 220 DEG C, 215 DEG C, 215 DEG C from feeding section to head, screw speed is 200 revs/min, and screw slenderness ratio is 44.Its flame retardant properties is in Table-3.
comparative example 10
Be the ABS DG417 of 100 parts by weight part, the fire retardant B of 13 parts, the fire retardant E of 5 parts, the fire retardant D of 5 parts, 0.2 part of oxidation inhibitor C, 0.3 part of oxidation inhibitor D, 0.25 part of Lubricate EBS, 0.15 part of steady agent A of light, 0.15 part of steady agent B of light add in high-speed mixer and mix.Wherein, the temperature of high-speed mixer is that 70 DEG C, the speed of high-speed mixer are 120 revs/min.Then the material mixing is added in twin screw extruder extrude, cooling, granulation, dress bag.The temperature of forcing machine is followed successively by 200 DEG C, 225 DEG C, 225 DEG C, 220 DEG C, 220 DEG C, 220 DEG C, 215 DEG C, 215 DEG C from feeding section to head, screw speed is 200 revs/min, and screw slenderness ratio is 44.Its flame retardant properties is in Table-3.
embodiment 9
Be the ABS DG417 of 100 parts by weight part, the fire retardant B of 13 parts, the fire retardant E of 5 parts, the fire retardant D of 10 parts, the double-walled carbon nano-tube A of 0.9 part, 0.2 part of oxidation inhibitor C, 0.3 part of oxidation inhibitor D, 0.25 part of Lubricate EBS, 0.15 part of steady agent A of light, 0.15 part of steady agent B of light add in high-speed mixer and mix.Wherein, the temperature of high-speed mixer is that 70 DEG C, the speed of high-speed mixer are 120 revs/min.Then the material mixing is added in twin screw extruder extrude, cooling, granulation, dress bag.The temperature of forcing machine is followed successively by 200 DEG C, 225 DEG C, 225 DEG C, 220 DEG C, 220 DEG C, 220 DEG C, 215 DEG C, 215 DEG C from feeding section to head, screw speed is 200 revs/min, and screw slenderness ratio is 44.Its flame retardant properties is in Table-3.
comparative example 11
Be the ABS DG417 of 100 parts by weight part, the fire retardant B of 13 parts, the fire retardant E of 5 parts, the fire retardant D of 10 parts, 0.2 part of oxidation inhibitor C, 0.3 part of oxidation inhibitor D, 0.25 part of Lubricate EBS, 0.15 part of steady agent A of light, 0.15 part of steady agent B of light add in high-speed mixer and mix.Wherein, the temperature of high-speed mixer is that 70 DEG C, the speed of high-speed mixer are 120 revs/min.Then the material mixing is added in twin screw extruder extrude, cooling, granulation, dress bag.The temperature of forcing machine is followed successively by 200 DEG C, 225 DEG C, 225 DEG C, 220 DEG C, 220 DEG C, 220 DEG C, 215 DEG C, 215 DEG C from feeding section to head, screw speed is 200 revs/min, and screw slenderness ratio is 44.Its flame retardant properties is in Table-3.
comparative example 12
Be the ABS DG417 of 100 parts by weight part, the fire retardant B of 13 parts, the fire retardant E of 5 parts, the fire retardant D of 10 parts, the anti-dripping agent PTF-5050 of 0.9 part, 0.2 part of oxidation inhibitor C, 0.3 part of oxidation inhibitor D, 0.25 part of Lubricate EBS, 0.15 part of steady agent A of light, 0.15 part of steady agent B of light add in high-speed mixer and mix.Wherein, the temperature of high-speed mixer is that 70 DEG C, the speed of high-speed mixer are 120 revs/min.Then the material mixing is added in twin screw extruder extrude, cooling, granulation, dress bag.The temperature of forcing machine is followed successively by 200 DEG C, 225 DEG C, 225 DEG C, 220 DEG C, 220 DEG C, 220 DEG C, 215 DEG C, 215 DEG C from feeding section to head, screw speed is 200 revs/min, and screw slenderness ratio is 44.Its flame retardant properties is in Table-3.
The flame retardant properties of table-3 embodiment 7-9 and comparative example 9 ~ 12
| Test event | Embodiment 7 | Comparative example 9 | Embodiment 8 | Comparative example 10 | Embodiment 9 | Comparative example 11 | Comparative example 12 |
| UL-94 flame retardant rating | V0 | V0 | V0 | V0 | V0 | V0 | V0 |
| The t1+t2 summation (second) of 5 battens | 0 | 6 | 2 | 13 | 2 | 11 | 6 |
From above embodiment 7 ~ 9 and comparative example 9 ~ 11, can obviously find out, add carbon nanotube of the present invention to use as anti-dripping agent effective more a lot of than not adding; Can obviously find out from embodiment 7 and comparative example 9, the t1+t2 summation that adds 5 samples of carbon nanotube is 0 second, and the t1+t2 summation that does not add 5 samples of carbon nanotube is 6 seconds.On the other hand, from embodiment 9, comparative example 11 and comparative example 12 relatively can find out, the in the situation that of same amount, anti-dripping agent of the present invention is more effective than traditional PTFE type anti-dripping agent.
embodiment 10
Be the PA6 M2500 of 100 parts by weight part, the fire retardant A of 18 parts, the fire retardant E of 7 parts, the multi-walled carbon nano-tubes A of 0.75 part, 0.2 part of oxidation inhibitor B, 0.3 part of oxidation inhibitor D, 0.25 part of Lubricate EBS, 0.15 part of steady agent A of light, 0.15 part of steady agent B of light add in high-speed mixer and mix.Wherein, the temperature of high-speed mixer is that 70 DEG C, the speed of high-speed mixer are 120 revs/min.Then the material mixing is added in twin screw extruder extrude, cooling, granulation, dress bag.The temperature of forcing machine is followed successively by 200 DEG C, 225 DEG C, 225 DEG C, 220 DEG C, 220 DEG C, 220 DEG C, 215 DEG C, 215 DEG C from feeding section to head, screw speed is 200 revs/min, and screw slenderness ratio is 44.Its flame retardant properties is in Table-4.
comparative example 13
Be the PA6 M2500 of 100 parts by weight part, the fire retardant A of 18 parts, the fire retardant E of 7 parts, 0.2 part of oxidation inhibitor B, 0.3 part of oxidation inhibitor D, 0.25 part of Lubricate EBS, 0.15 part of steady agent A of light, 0.15 part of steady agent B of light add in high-speed mixer and mix.Wherein, the temperature of high-speed mixer is that 70 DEG C, the speed of high-speed mixer are 120 revs/min.Then the material mixing is added in twin screw extruder extrude, cooling, granulation, dress bag.The temperature of forcing machine is followed successively by 200 DEG C, 225 DEG C, 225 DEG C, 220 DEG C, 220 DEG C, 220 DEG C, 215 DEG C, 215 DEG C from feeding section to head, screw speed is 200 revs/min, and screw slenderness ratio is 44.Its flame retardant properties is in Table-4.
embodiment 11
Be the PET CB-608S of 100 parts by weight part, the fire retardant B of 18 parts, the fire retardant E of 7 parts, the Single Walled Carbon Nanotube B of 0.45 part, 0.2 part of oxidation inhibitor C, 0.3 part of oxidation inhibitor D, 0.25 part of Lubricate EBS, 0.15 part of steady agent A of light, 0.15 part of steady agent B of light add in high-speed mixer and mix.Wherein, the temperature of high-speed mixer is that 70 DEG C, the speed of high-speed mixer are 120 revs/min.Then the material mixing is added in twin screw extruder extrude, cooling, granulation, dress bag.The temperature of forcing machine is followed successively by 240 DEG C, 275 DEG C, 275 DEG C, 270 DEG C, 270 DEG C, 270 DEG C, 265 DEG C, 265 DEG C from feeding section to head, screw speed is 200 revs/min, and screw slenderness ratio is 44.Its flame retardant properties is in Table-4.
comparative example 14
Be the PET CB-608S of 100 parts by weight part, the fire retardant B of 18 parts, the fire retardant E of 7 parts, 0.2 part of oxidation inhibitor C, 0.3 part of oxidation inhibitor D, 0.25 part of Lubricate EBS, 0.15 part of steady agent A of light, 0.15 part of steady agent B of light add in high-speed mixer and mix.Wherein, the temperature of high-speed mixer is that 70 DEG C, the speed of high-speed mixer are 120 revs/min.Then the material mixing is added in twin screw extruder extrude, cooling, granulation, dress bag.The temperature of forcing machine is followed successively by 240 DEG C, 275 DEG C, 275 DEG C, 270 DEG C, 270 DEG C, 270 DEG C, 265 DEG C, 265 DEG C from feeding section to head, screw speed is 200 revs/min, and screw slenderness ratio is 44.Its flame retardant properties is in Table-4.
The flame retardant properties of table-4 embodiment 10-11 and comparative example 13 ~ 14
| Test event | Embodiment 10 | Comparative example 13 | Embodiment 11 | Comparative example 14 |
| UL-94 flame retardant rating | V0 | V0 | V0 | V0 |
| The t1+t2 summation (second) of 5 battens | 0 | 7 | 0 | 6 |
From above embodiment 10 ~ 11 and comparative example 13 ~ 14, can obviously find out, add carbon nanotube of the present invention to use as anti-dripping agent effective more a lot of than not adding; Can obviously find out from embodiment 10 and comparative example 13, the t1+t2 summation that adds 5 samples of carbon nanotube is 0 second, and the t1+t2 summation that does not add 5 samples of carbon nanotube is 7 seconds.
Can obviously find out from above all embodiment and all comparative examples, the present invention uses carbon nanotube as anti-dripping agent, and its effect is remarkable, than not adding anti-dripping agent good flame retardation effect, and might as well than adding traditional anti-dripping agent flame retardant effect.
Claims (10)
1. carbon nanotube is as a purposes for composition flame-retardant anti-dropping agent, and described carbon nanotube is that surface does not have the carbon nanotube of modification or for the carbon nanotube of surface hydroxylation or be the carboxylated carbon nanotube in surface.
2. a kind of carbon nanotube, as the purposes of composition flame-retardant anti-dropping agent, is characterized in that as claimed in claim 1, and described carbon nanotube is Single Walled Carbon Nanotube, and its external diameter 1 ~ 2 nanometer, length are at 5 ~ 30 microns, purity > 90wt%.
As claimed in claim 1 a kind of carbon nanotube as the purposes of composition flame-retardant anti-dropping agent, it is characterized in that, described carbon nanotube is multi-walled carbon nano-tubes, and its external diameter < 8 nanometers, length are at 10 ~ 30 microns, purity > 98wt%.
4. as claimed in claim 1, a kind of carbon nanotube, as the purposes of composition flame-retardant anti-dropping agent, is characterized in that, described carbon nanotube is double-walled carbon nano-tube, and its external diameter 2 ~ 4 nanometers, length are at 5 ~ 15 microns, purity > 60wt%.
5. a kind of carbon nanotube, as the purposes of composition flame-retardant anti-dropping agent, is characterized in that as claimed in claim 1, and the hydroxy radical content of the carbon nanotube of described surface hydroxylation is at 3.8wt% ~ 5.8wt%.
6. a kind of carbon nanotube, as the purposes of composition flame-retardant anti-dropping agent, is characterized in that as claimed in claim 1, and the carboxyl-content of the carboxylated carbon nanotube in described surface is at 2.7wt% ~ 3.9wt%.
7. a kind of carbon nanotube, as the purposes of composition flame-retardant anti-dropping agent, is characterized in that as claimed in claim 1: the body material in described composition is polyethylene, polypropylene, polymeric amide, polycarbonate, acrylonitrile-butadiene-styrene resin, polyethylene terephthalate or polybutylene terephthalate.
8. a kind of carbon nanotube, as the purposes of composition flame-retardant anti-dropping agent, is characterized in that described body material polymeric amide is one or more in polyamide 6, polyamide 66, polyamide 610, polymeric amide 46, polyamide 1010, polyamide 612, polymeric amide 12, polymeric amide 8, polymeric amide 9 as claimed in claim 7.
9. as described in claim 7 or 8, carbon nanotube, as the purposes of composition flame-retardant anti-dropping agent, is characterized in that: in described composition, the consumption of carbon nanotube is the 0.1%-1% of composition substrate quality of materials.
As claimed in claim 9 carbon nanotube as the purposes of composition flame-retardant anti-dropping agent, it is characterized in that: in described composition, taking composition substrate quality of materials as benchmark, also include 12wt% ~ 30wt% fire retardant, 0.2wt% ~ 0.5wt% oxidation inhibitor, 0.1wt% ~ 0.3wt% lubricant and the steady agent of 0.1wt% ~ 0.3wt% light.
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| CN106750053A (en) * | 2016-12-19 | 2017-05-31 | 衢州普信新材料有限公司 | A kind of preparation method of CNT Antidrip agent |
| CN107663366A (en) * | 2016-07-27 | 2018-02-06 | 汉达精密电子(昆山)有限公司 | CNT strengthens halogen-free flame retardant PC/ABS composite material and its products formed |
| CN107915980A (en) * | 2017-11-23 | 2018-04-17 | 清远初曲智能科技有限公司 | A kind of methylolation flame-retardant polycarbonate material and preparation method thereof |
| CN108276749A (en) * | 2017-12-19 | 2018-07-13 | 宁波甬尚聚新材料有限公司 | A kind of halogen-free flame retardants and the resin alloy containing the halogen-free flame retardants |
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| CN111117183A (en) * | 2019-12-12 | 2020-05-08 | 上海普利特复合材料股份有限公司 | Antistatic, low-smoke, halogen-free and flame-retardant PC/ABS blending material and preparation method thereof |
| CN112679916A (en) * | 2020-12-09 | 2021-04-20 | 金发科技股份有限公司 | PBT composition and preparation method and application thereof |
| CN112852121A (en) * | 2020-12-31 | 2021-05-28 | 东莞市基烁实业有限公司 | Conductive master batch for PET (polyethylene terephthalate) sheet as well as preparation method and application thereof |
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| CN105155252A (en) * | 2015-09-18 | 2015-12-16 | 浙江理工大学 | Fabric provided with flame-retardant coatings including carbon nano tubes on surfaces and preparation method thereof |
| CN105155252B (en) * | 2015-09-18 | 2018-01-12 | 浙江理工大学 | Fabric of surface carbon nanotubes flame retardant coating and preparation method thereof |
| CN107663366A (en) * | 2016-07-27 | 2018-02-06 | 汉达精密电子(昆山)有限公司 | CNT strengthens halogen-free flame retardant PC/ABS composite material and its products formed |
| CN106750053A (en) * | 2016-12-19 | 2017-05-31 | 衢州普信新材料有限公司 | A kind of preparation method of CNT Antidrip agent |
| CN107915980A (en) * | 2017-11-23 | 2018-04-17 | 清远初曲智能科技有限公司 | A kind of methylolation flame-retardant polycarbonate material and preparation method thereof |
| CN108276749A (en) * | 2017-12-19 | 2018-07-13 | 宁波甬尚聚新材料有限公司 | A kind of halogen-free flame retardants and the resin alloy containing the halogen-free flame retardants |
| CN108586939B (en) * | 2018-05-24 | 2020-09-11 | 龙岩市润峰科技有限公司 | Environment-friendly flame-retardant conductive polypropylene material |
| CN108586939A (en) * | 2018-05-24 | 2018-09-28 | 暨南大学 | A kind of environmental protection flame retardant conductive polypropylene material |
| CN111117183A (en) * | 2019-12-12 | 2020-05-08 | 上海普利特复合材料股份有限公司 | Antistatic, low-smoke, halogen-free and flame-retardant PC/ABS blending material and preparation method thereof |
| CN112679916A (en) * | 2020-12-09 | 2021-04-20 | 金发科技股份有限公司 | PBT composition and preparation method and application thereof |
| CN112679916B (en) * | 2020-12-09 | 2022-04-19 | 金发科技股份有限公司 | PBT composition and preparation method and application thereof |
| CN112852121A (en) * | 2020-12-31 | 2021-05-28 | 东莞市基烁实业有限公司 | Conductive master batch for PET (polyethylene terephthalate) sheet as well as preparation method and application thereof |
| CN113861653A (en) * | 2021-09-28 | 2021-12-31 | 上海金发科技发展有限公司 | Flame-retardant polycarbonate composite material and preparation method and application thereof |
| CN113861653B (en) * | 2021-09-28 | 2023-09-12 | 上海金发科技发展有限公司 | Flame-retardant polycarbonate composite material and preparation method and application thereof |
| CN114621573A (en) * | 2022-03-15 | 2022-06-14 | 金发科技股份有限公司 | Halogen-free flame-retardant carbon fiber reinforced polycarbonate composition and preparation method and application thereof |
| CN114621573B (en) * | 2022-03-15 | 2023-06-23 | 金发科技股份有限公司 | Halogen-free flame-retardant carbon fiber reinforced polycarbonate composition and preparation method and application thereof |
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