CN104693782A - Halogen-free flame retardant polyether thermoplastic polyurethane elastomer and preparation method thereof - Google Patents
Halogen-free flame retardant polyether thermoplastic polyurethane elastomer and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a halogen-free flame retardant polyether thermoplastic polyurethane elastomer which is prepared by the following components in parts by weight: 100 parts of polyether thermoplastic polyurethane elastomer resin, 30-50 parts of phosphor-nitrogen flame retardant system and 1-5 parts of flame retardant synergist, wherein the phosphor-nitrogen flame retardant system is prepared by mixing a flame retardant and a char-forming agent with weight ratio of 1-4: 1; and the flame retardant is one or a mixture of phenoxy cycloposphazene, melamine phosphate compound, melamine cyanurate and hypophosphite. The flame retardant performance of the polyether TPU (thermoplastic polyurethane) is modified by selecting the special phosphor-nitrogen flame retardant system; and the obtained flame retardant polyether TPU material is halogen-free, environment-friendly and safe, has a limit oxygen index (LOI) of up to 37% and has excellent flame retardant performance.
Description
Technical field
the invention belongs to technical field of polymer materials, be specifically related to a kind of halogen-free flameproof Polyether-type thermoplastic polyurethane elastomer and preparation method thereof.
Background technology
polyurethane Thermoplastic Elastomer (TPU, Thermoplastic polyurethane) mainly contain polyester type and polyether-type point.Polyether-type TPU has the advantages such as high strength, hydrolysis, high resilience and low-temperature performance are good, is widely used in and produces electric wire and cable jacket, motion climbing boot material, fire-proof and thermal-insulation sound-proof material and multi-function membrane etc.The weak point of polyether-type TPU is that it belongs to inflammable material, oxygen index only about 18%, and has dense smoke and disengage and serious molten drop with a large amount of obnoxious flavour during burning, therefore needs to carry out it flame-retardant modified to meet application requiring.
current commercial flame retarding polyether type TPU mainly adopt bromide fire retardant and metal hydroxide combustion inhibitor fire-retardant to carry out, but there is environmental issue because of halogen-containing in bromide fire retardant; Metal hydroxide combustion inhibitor addition is large, to the surface of TPU goods and Effect on Mechanical Properties larger.
Summary of the invention
the present invention is intended to overcome shortcoming of the prior art, provides the halogen-free flameproof Polyether-type thermoplastic polyurethane elastomer that a kind of environmental protection, flame retardant properties and mechanical property are good.
another object of the present invention is to provide the preparation method of above-mentioned halogen-free flameproof Polyether-type thermoplastic polyurethane elastomer.
for solving above technical problem, the technical scheme that the present invention takes is:
a kind of halogen-free flameproof Polyether-type thermoplastic polyurethane elastomer, by weight, its feed composition comprises:
polyether-type thermoplastic polyurethane elastomer resin 100 parts
phosphorus nitrogen flame-retardant system 30 ~ 50 parts
retardant synergist 1 ~ 5 part
0.5 ~ 2 part, oxidation inhibitor
surface-modifying agent 0.5 ~ 2 part
coupling agent 0.5 ~ 2 part
lubricant 0.5 ~ 4 part
wherein, described phosphorus nitrogen flame-retardant system is mixed by fire retardant and the char-forming agent ratio by weight 1 ~ 4:1, and described fire retardant is the combination of one or more in phenoxy group ring phosphonitrile, trimeric cyanamide phosphate compound, melamine cyanurate and secondary phosphorus (phosphine) hydrochlorate.
preferably, described trimeric cyanamide phosphate compound is the combination of one or more in melamine phosphate (MP), melamine polyphosphate (MPP) and melamine pyrophosphate (MPOP).
preferably, described secondary phosphorus (phosphine) hydrochlorate is that hypophosphite, diethyl phosphinates are (as diethyl hypo-aluminum orthophosphate, ADP) combination of one or more, in phenyl phosphinic acid salt (as phenyl hypo-aluminum orthophosphate, AIPP), methylcyclohexyl phosphinates, hydroxyalkylphenyl phosphinates and Phospholes phosphinates.
preferably, described char-forming agent is the combination of one or more in tetramethylolmethane young laying ducks in cage (PEPA), tetramethylolmethane (PER), dipentaerythritol (DPER), triazine char-forming agent and piperazine pyrophosphate.
preferably, described retardant synergist is the combination of one or more in Resorcinol (diphenyl phosphoester) (i.e. RDP), dihydroxyphenyl propane two (diphenyl phosphoester) (i.e. BDP), phosphate toluene diphenyl ester (i.e. CDP), magnesium oxide, hydrotalcite and aluminium titanates.
preferably, described oxidation inhibitor is the combination of one or more in irgasfos 168, antioxidant 1010 and oxidation inhibitor B215,
preferably, described coupling agent is the combination of one or more in silane coupling agent, titanate coupling agent and aluminate coupling agent.
preferably, described surface-modifying agent is multi-polysiloxane, as selected DOW CORNING 11-100 or DOW CORNING Z-6173.
preferably, described lubricant is the combination of one or more in silicone powder, silicone master batch, Zinic stearas, calcium stearate, polyethylene wax, maleic anhydride grafted polyethylene wax, pentaerythritol stearate and ethylene bis stearamide (i.e. EBS).
the preparation method of above-mentioned halogen-free flameproof Polyether-type thermoplastic polyurethane elastomer, comprises the steps:
(1) Polyether-type thermoplastic polyurethane elastomer resin and retardant synergist is even in high-speed mixer and mixing, period sprays into surface-modifying agent by the spray equipment that high mixer inner core is arranged, and makes material carry out surface modification while high-speed mixing;
(2) phosphorus nitrogen flame-retardant system, oxidation inhibitor, coupling agent and lubricant are added high-speed mixer and mixing even;
(3) from main charging opening, the material of step (1) gained is added twin screw extruder, and the material of step (2) gained adds from the side spout of twin screw extruder, controlled working temperature is between 160 DEG C ~ 190 DEG C, carry out melt blending, extruding pelletization, obtain described halogen-free flameproof Polyether-type thermoplastic polyurethane elastomer.
due to the enforcement of above technical scheme, the present invention compared with prior art tool has the following advantages:
the present invention carries out flame-retardant modified by selecting specific phosphorus nitrogen flame-retardant system to polyether-type TPU, and the flame retarding polyether type TPU material obtained is not halogen-containing, Environmental Safety, and limiting oxygen index(LOI) LOI value can reach 37%, has excellent flame retardant properties.First the inventive method carries out modification with surface-modifying agent and retardant synergist to TPU particle surface, then by the mode of side feeding, other pulvis such as fire retardant, coupling agent are joined in twin screw extruder, carry out melt blending again with the TPU particle of modification to extrude, enable the flame retarding polyether type TPU elastomerics of gained better keep its mechanical property, excellent flame retardant properties can be obtained again simultaneously.
Embodiment
below in conjunction with embodiment, the present invention will be further described in detail, but be not limited to these embodiments.
halogen-free flameproof polyether-type TPU elastomerics of the present invention is prepared from by following working method:
(1) by TPU particle and retardant synergist (being generally liquid or powder) in high mixer with the rotating speed high-speed mixing 5 ~ 10min of 1000r/min, period sprays into surface-modifying agent by the spray equipment that high mixer inner core is arranged, and makes material carry out surface modification while high-speed mixing;
(2) phosphorus nitrogen flame-retardant system, oxidation inhibitor, coupling agent and lubricant are added in high mixer, with the rotating speed high-speed mixing 10 ~ 15min of 1400r/min;
(3) from main charging opening, the material of step (1) gained is added twin screw extruder, and the material of step (2) gained adds from the side spout of twin screw extruder, controlled working temperature is between 160 DEG C ~ 190 DEG C, carry out melt blending to extrude, and pass through the mode granulation of underwater cutpellet, obtain halogen-free flameproof polyether-type TPU elastomer material of the present invention.
embodiment 1
it is as follows that the present embodiment prepares the elastomeric composition of raw materials of halogen-free flameproof polyether-type TPU:
100 parts, TPU particle
melamine polyphosphate (MPP) 20 parts
methylcyclohexyl phosphinates 10 parts
piperazine pyrophosphate 10 parts
2 parts, magnesium oxide
dOW CORNING 11-100 0.5 part
irgasfos 168 0.5 part
antioxidant 1010 1 part
silane coupling agent 1 part
silicone powder 0.5 part
embodiment 2
it is as follows that the present embodiment prepares the elastomeric composition of raw materials of halogen-free flameproof polyether-type TPU:
100 parts, TPU particle
aluminum diethylphosphinate (ADP) 20 parts
melamine cyanurate (MCA) 10 parts
tetramethylolmethane 10 parts
triazine char-forming agent 5 parts
hydrotalcite 1 part
resorcinol (diphenyl phosphoester) (RDP) 1 part
dOW CORNING 11-100 0.5 part
oxidation inhibitor B215 1.5 parts
silane coupling agent 0.5 part
silicone powder 0.5 part
embodiment 3
it is as follows that the present embodiment prepares the elastomeric composition of raw materials of halogen-free flameproof polyether-type TPU:
100 parts, TPU particle
phenyl hypo-aluminum orthophosphate (AIPP) 20 parts
melamine cyanurate (MCA) 10 parts
tetramethylolmethane young laying ducks in cage (PEPA) 8 parts
dipentaerythritol 7 parts
hydrotalcite 1 part
resorcinol (diphenyl phosphoester) (RDP) 1 part
dOW CORNING 11-100 0.5 part
oxidation inhibitor B215 1 part
aluminate coupling agent 0.5 part
zinic stearas 0.5 part
embodiment 4
it is as follows that the present embodiment prepares the elastomeric composition of raw materials of halogen-free flameproof polyether-type TPU:
100 parts, TPU particle
phenoxy group ring phosphonitrile 10 parts
melamine pyrophosphate (MPOP) 10 parts
piperazine pyrophosphate 10 parts
tetramethylolmethane 10 parts
aluminium titanates 2 parts
dOW CORNING Z-6173 0.5 part
irgasfos 168 0.5 part
antioxidant 1010 1 part
titanate coupling agent 0.5 part
silicone powder 0.5 part
embodiment 5
it is as follows that the present embodiment prepares the elastomeric composition of raw materials of halogen-free flameproof polyether-type TPU:
100 parts, TPU particle
aluminum diethylphosphinate (ADP) 15 parts
melamine cyanurate (MCA) 10 parts
melamine polyphosphate (MPP) 5 parts
triazine char-forming agent 7 parts
tetramethylolmethane young laying ducks in cage (PEPA) 8 parts
2 parts, magnesium oxide
hydrotalcite 1 part
dOW CORNING 11-100 0.5 part
oxidation inhibitor B215 1 part
silane coupling agent 0.5 part
calcium stearate 0.5 part
embodiment 6
it is as follows that the present embodiment prepares the elastomeric composition of raw materials of halogen-free flameproof polyether-type TPU:
100 parts, TPU particle
phenyl hypo-aluminum orthophosphate (AIPP) 15 parts
melamine polyphosphate (MPP) 10 parts
melamine pyrophosphate (MPOP) 5 parts
tetramethylolmethane young laying ducks in cage (PEPA) 10 parts
hydrotalcite 1 part
resorcinol (diphenyl phosphoester) (RDP) 1 part
dOW CORNING Z-6173 0.5 part
oxidation inhibitor B215 1 part
aluminate coupling agent 0.5 part
silicone powder 0.5 part
embodiment 7
it is as follows that the present embodiment prepares the elastomeric composition of raw materials of halogen-free flameproof polyether-type TPU:
100 parts, TPU particle
hydroxyalkylphenyl phospho acid 15 parts
melamine cyanurate (MCA) 10 parts
phenoxy group ring phosphonitrile 5 parts
dipentaerythritol 10 parts
piperazine pyrophosphate 5 parts
hydrotalcite 1 part
dOW CORNING 11-100 0.5 part
irgasfos 168 0.5 part
antioxidant 1010 1 part
silane coupling agent 0.5 part
silicone powder 0.5 part
embodiment 8
carry out flame retardant properties test to the above-mentioned TPU material obtained by the composition of raw materials processing in embodiment 1 ~ 7, result is see table-1.
testing standard:
limiting oxygen index(LOI) (LOI) test is with reference to ASTM D2863 standard;
uL-94 standard;
electric wire wire rod flame retardant test vw-1 is with reference to UL1581 standard;
table-1
as can be seen from table-1, halogen-free flameproof polyether-type TPU elastomer material of the present invention has extraordinary flame retardant effect, and UL-94 test all can reach V-0 rank, and limiting oxygen index(LOI) all can reach more than 33%, reach as high as 37%, and all can be tested by vw-1.
above to invention has been detailed description; its object is to allow the personage being familiar with this art can understand content of the present invention and be implemented; can not limit the scope of the invention with this; the equivalence change that all spirit according to the present invention are done or modification, all should be encompassed in protection scope of the present invention.
Claims (10)
1. a halogen-free flameproof Polyether-type thermoplastic polyurethane elastomer, is characterized in that: by weight, and its material component comprises:
Polyether-type thermoplastic polyurethane elastomer resin 100 parts
Phosphorus nitrogen flame-retardant system 30 ~ 50 parts
Retardant synergist 1 ~ 5 part
0.5 ~ 2 part, oxidation inhibitor
Surface-modifying agent 0.5 ~ 2 part
Coupling agent 0.5 ~ 2 part
Lubricant 0.5 ~ 4 part
Wherein, described phosphorus nitrogen flame-retardant system is mixed by fire retardant and the char-forming agent ratio by weight 1 ~ 4:1, and described fire retardant is the combination of one or more in phenoxy group ring phosphonitrile, trimeric cyanamide phosphate compound, melamine cyanurate and secondary phosphorus (phosphine) hydrochlorate.
2. halogen-free flameproof Polyether-type thermoplastic polyurethane elastomer according to claim 1, is characterized in that: described trimeric cyanamide phosphate compound is the combination of one or more in melamine phosphate, melamine polyphosphate and melamine pyrophosphate.
3. halogen-free flameproof Polyether-type thermoplastic polyurethane elastomer according to claim 1, is characterized in that: described secondary phosphorus (phosphine) hydrochlorate is the combination of one or more in hypophosphite, diethyl phosphinates, phenyl phosphinic acid salt, methylcyclohexyl phosphinates, hydroxyalkylphenyl phosphinates and Phospholes phosphinates.
4. halogen-free flameproof Polyether-type thermoplastic polyurethane elastomer according to claim 1, is characterized in that: described char-forming agent is the combination of one or more in tetramethylolmethane young laying ducks in cage, tetramethylolmethane, dipentaerythritol, triazine char-forming agent and piperazine pyrophosphate.
5. halogen-free flameproof Polyether-type thermoplastic polyurethane elastomer according to claim 1, is characterized in that: described retardant synergist is the combination of one or more in Resorcinol (diphenyl phosphoester), dihydroxyphenyl propane two (diphenyl phosphoester), phosphate toluene diphenyl ester, magnesium oxide, hydrotalcite and aluminium titanates.
6. halogen-free flameproof Polyether-type thermoplastic polyurethane elastomer according to claim 1, is characterized in that: described oxidation inhibitor is the combination of one or more in irgasfos 168, antioxidant 1010 and oxidation inhibitor B215.
7. halogen-free flameproof Polyether-type thermoplastic polyurethane elastomer according to claim 1, is characterized in that: described coupling agent is the combination of one or more in silane coupling agent, titanate coupling agent and aluminate coupling agent.
8. halogen-free flameproof Polyether-type thermoplastic polyurethane elastomer according to claim 1, is characterized in that: described surface-modifying agent is multi-polysiloxane.
9. halogen-free flameproof Polyether-type thermoplastic polyurethane elastomer according to claim 1, is characterized in that: described lubricant is the combination of one or more in silicone powder, silicone master batch, Zinic stearas, calcium stearate, polyethylene wax, maleic anhydride grafted polyethylene wax, pentaerythritol stearate and ethylene bis stearamide.
10. the preparation method of the halogen-free flameproof Polyether-type thermoplastic polyurethane elastomer according to any one of claim 1 ~ 9, is characterized in that: comprise the steps:
(1) Polyether-type thermoplastic polyurethane elastomer resin and retardant synergist is even in high-speed mixer and mixing, period sprays into surface-modifying agent by the spray equipment that high mixer inner core is arranged, and makes material carry out surface modification while high-speed mixing;
(2) phosphorus nitrogen flame-retardant system, oxidation inhibitor, coupling agent and lubricant are added high-speed mixer and mixing even;
(3) from main charging opening, the material of step (1) gained is added twin screw extruder, and the material of step (2) gained adds from the side spout of twin screw extruder, controlled working temperature is between 160 DEG C ~ 190 DEG C, carry out melt blending, extruding pelletization, obtain described halogen-free flameproof Polyether-type thermoplastic polyurethane elastomer.
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