CN108299803A - A kind of transparent PET material of high fire-retardance and preparation method thereof - Google Patents
A kind of transparent PET material of high fire-retardance and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to technical field of polymer materials, and in particular to a kind of transparent PET material of high fire-retardance and preparation method thereof, which includes the raw material of following parts by weight：70 118 parts of PET resins, 8 16 portions of nucleating agents, 37 parts of compatilizers, 7 13 parts of fire retardants, 13 portions of synergist, 0.5 1.0 parts of talcum powder and 26 parts of coupling agents, the nucleating agent is by 2,2 ' di-2-ethylhexylphosphine oxides (4,6 t-butyl phenol) phosphine aluminium salt, dibenzal sorbitol and two (replacing benzal to chlorine) sorbierites are with weight ratio for 2.5 3.5:1.2‑1.8:The mixture of 0.8 1.2 compositions.The transparent PET material transparent of the present invention is visual, and with performances such as preferable transparency, anti-flammability, heat resistance, smoke-suppressing, stability, anti-oxidant agings, intensity is high, and processability is good, and processing performance is good, and use value is high.
Description
Technical field
The present invention relates to technical field of polymer materials, and in particular to a kind of transparent PET material of high fire-retardance and its preparation
Method.
Background technology
It is fast-developing with the power domain in China, it is various applied to the pipe material in electric power protection at present, and electric power
Protection pipe is the important original paper in power domain, and excellent protective effect is played to the electric power material such as electric wire, light, cable, more
Using materials such as PET, PVC, PE, PP, wherein PET material is since its wearability is good, plasticity is strong, solvent resistance is good, resistance to surface
Scrape the features such as damage property is good, crack resistance is good, mechanical and physical performance is good and extensive use, but the melt strength of PET material, dimensionally stable
There are still deficiencies for the performances such as property, barrier property, heat resistance；In addition, current electric power protection tubing is mostly the tubing of multiple color
Material, the case where being difficult in practical application understand electric wire in pipe in real time by tubing, practicability is relatively low.
Invention content
In order to overcome shortcoming and defect existing in the prior art, the purpose of the present invention is to provide a kind of the saturating of high fire-retardance
Bright PET material, the transparent PET material transparent is visual, and with preferable transparency, anti-flammability, heat resistance, smoke-suppressing, stabilization
Property, the performances such as anti-oxidant aging, intensity is high, and processability is good, and processing performance is good, and use value is high.
Another object of the present invention is to provide a kind of preparation method of the transparent PET material of high fire-retardance, the preparation methods
Simply, convenient operation and control, stable quality, production efficiency is high, and production cost is low, is suitble to large-scale industrial production.
The purpose of the invention is achieved by the following technical solution：A kind of transparent PET material of high fire-retardance, the transparent PET material
Material includes the raw material of following parts by weight：
The nucleating agent is (right by 2,2 '-di-2-ethylhexylphosphine oxides (4,6- t-butyl phenol) phosphine aluminium salt, dibenzal sorbitol and two
Chlorine replaces benzal) sorbierite with weight ratio is 2.5-3.5:1.2-1.8:The mixture of 0.8-1.2 compositions.
The transparent PET material of the present invention by using above-mentioned raw materials, between each raw material mutual cooperation act on, concerted reaction,
It can make transparent PET material obtained that there is preferable transparency, anti-flammability, heat resistance, smoke-suppressing, stability, anti-oxidant aging
Etc. performances, intensity it is high, processability is good, and processing performance is good；Wherein, it mutually acts synergistically with synergist by using fire retardant, both
Flame retardant effect can be improved, and smoke suppressing effect can be played；By using 2,2 '-di-2-ethylhexylphosphine oxides (4,6- t-butyl phenol) phosphine aluminium salt,
Dibenzal sorbitol and two (replacing benzal to chlorine) sorbierites strictly control the mixed proportion of three as heat-resistant filler, can
Accelerate crystalline rate, increase crystal density and promote fine grain size, shorten molding cycle, improves transparent PET material
The physical mechanical properties such as the transparency, tensile strength, rigidity, heat distortion temperature, impact resistance, creep resistance, lustrous surface can have
The case where helping understand electric wire in pipe in real time by tubing, practicability are high.
Preferably, the compatilizer is haloflex, Methylacrylate-Acrylate Copolymer, two Malaysia of penylene
Acid imide, natural gum grafting polymethyl methacrylate, styrene-grafted maleic anhydride and ethylene-acrylic acid-butyl ester are grafted first
At least one of base glycidyl acrylate.
The transparent PET material of the present invention by using mentioned kind as compatilizer, can be matched with other raw materials effect,
Concerted reaction effectively reduces PET intermolecular interfacial tensions when being reacted with other raw materials, and then raising interface cohesive force, makes point
Dephasing and continuous phase are uniform, form stable structure, promote the mutual cooperation reaction of each raw material of transparent PET material, improve transparent
The mechanical performances such as tensile strength, the impact strength of PET material improve rheological performance, improve surface smoothness.It is more highly preferred to
, the compatilizer is by Methylacrylate-Acrylate Copolymer, natural gum grafting polymethyl methacrylate and penylene
Dimaleimide is 1.6-2.4 with weight ratio：2.5-3.5:The mixture of 1 composition.
Preferably, the fire retardant be three (2,3- dibromopropyl) fulminuric acid esters, tribromphenol, aluminium triphosphate,
At least one in dimethyl methyl phosphonate, tetrabromobisphenol A bis- (2,3- dibromopropyl ethers), tetrabromophthalic anhydride and eight bromo ether
Kind.
The present invention by using mentioned kind fire retardant, it is environmentally friendly, can be matched with other raw materials effect, cooperate with it is anti-
It answers, and the flame retardant property of transparent PET material can be improved, the performance of transparent PET material is influenced smaller.More preferably, described
Fire retardant is by three (2,3- dibromopropyl) fulminuric acid ester, dimethyl methyl phosphonate and tetrabromophthalic anhydrides with weight
Than for 1.2-1.8:1:2.5-3.5 the mixture of composition.
Preferably, the synergist is antimony oxide, zinc stannate, zinc molybdate, magnesium silicate, zinc borate, zinc oxide and boron
At least one of sour zinc.
The present invention can match effect, concerted reaction by using the synergist of mentioned kind with other raw materials, and fire-retardant
Agent is matched with preferably synergistic effect, free radical can be captured in the gas phase, and play synergistic effect in condensed phase, transparent
PET material surface forms strong layer of charcoal, and then plays preferable fire-retardant, fireproofing function to transparent PET material, and plays suppression cigarette
Effect improves the color and luster of transparent PET material.More preferably, the synergist is by zinc stannate, zinc molybdate, magnesium silicate and boron
Sour zinc is 0.8-1.2 with weight ratio:1：1.0-1.5：2.4-3.2 the mixture of composition；The present invention is by using zinc stannate, molybdic acid
The compounding mixture of zinc, magnesium silicate and zinc borate has the antimony oxide more preferably synergistic than single use as synergist
Flame retardant effect.
Preferably, the coupling agent is vinyltriethoxysilane, anilinomethyl triethoxysilane, γ-methyl-prop
Alkene acryloxypropylethoxysilane trimethoxy silane, methyltriethoxysilane, pyrophosphate titanate esters and (the 'beta '-methoxy second of vinyl three
At least one of oxygroup) silane.
The present invention can match effect, concerted reaction with other raw materials, effectively carry by using the coupling agent of mentioned kind
High each raw pieces are combined closely, and heat resistance, dispersibility, cohesive force, anti-aging property, the intensity etc. of transparent PET material are improved
Comprehensive performance；Wherein, the vinyltriethoxysilane can effectively improve the affinity between each raw material, enhance transparent PET
The intensity of material；The γ-methacryloxypropyl trimethoxy silane improves the mechanical performance of transparent PET material, electricity
Gas performance, light transmission, ageing-resistant performance and weather resistance, bonding force is good, and durability is strong；The methyltriethoxysilane energy
Effectively improve the mechanical strength, heat resistance, humidity resistance of transparent PET material；The pyrophosphate titanate esters can effectively improve
The performances such as erosion-resisting characteristics, rheological characteristic, processability and the stability of transparent PET material；(the 'beta '-methoxy ethoxy of the vinyl three
Base) after silane combined with heat-resistant filler, the surface-hydrophobicized of heat-resistant filler can be made, and then improve heat-resistant filler and other raw materials
Compatibility achievees the effect that good dispersion, melt viscosity be low, excellent processing performance.More preferably, the coupling agent is γ-first
Base acryloyloxypropyltrimethoxysilane, methyltriethoxysilane and ('beta '-methoxy ethyoxyl) silane of vinyl three with
Weight ratio is 2.5-3.5:1:1.4-2.2 the mixture of composition.
Preferably, the transparent PET material further includes 1-5 parts of heat-resistant agents, the heat-resistant agent be magnesium silicide, ceramic fibre,
At least one of lignocellulosic, gas-phase silica and wollastonite in powder.
The present invention, as heat-resistant agent, effectively improves heat resistance, the processing flowing of transparent PET material by using above-mentioned raw materials
Performance reduces surface gloss, improves the comprehensive performance of M transparent PET finished materials.More preferably, the heat-resistant agent is pottery
Porcelain fiber, magnesium silicide and lignocellulosic are with weight ratio for 1:1.2-1.8:2.5-3.5 the mixture of composition.
Preferably, the transparent PET material further includes 0.5-2.5 parts of lubricants, and the lubricant is N, N ,-ethylenebis
Stearmide, oleamide, n-butyl stearate, three hydroxy stearic acid ester of glycerine, ethylene bis stearamide, stearmide, tristearin
At least one of sour zinc and oxidized polyethylene wax.
The present invention can match effect, concerted reaction by using the lubricant of mentioned kind with other raw materials, can be right
MPP tubing plays the role of preferable internal lubrication and external lubrication, reduces the active force between macromolecular, can be in molecule interface
The thin layer of lubrication is formed, and effectively reduces viscosity so that is easy to demould during post-processing, improves the stream of transparent PET material
Dynamic property, processability and processing performance；Wherein, there is the oxidized polyethylene wax lubrication and outer lubrication in preferably to make simultaneously
With, it is at low cost, and with the preferably transparency, the transparency of transparent PET material can be effectively improved.More preferably, the profit
Lubrication prescription is N, N, and-ethylenebisstearamide, stearmide and oxidized polyethylene wax are 0.8-1.2 with weight ratio:1：2.4-3.2
The mixture of composition.
Preferably, the transparent PET material further includes 2.4-3.2 parts of antioxidant, and the antioxidant is 2,6- di-t-butyls
Paracresol, 1,3,5- tri- (3,5 tertiary butyl-4-hydroxy benzyl) trimethylbenzenes, β-(3,5 di-tert-butyl-hydroxy phenyl) propionic acid
Octadecyl, 1,3,5- tri- (3,5 di-tert-butyl-hydroxy phenyl) isocyanates, three (2,4- di-tert-butyl-phenyl) phosphorous acid
At least one of ester, thiodipropionic acid dilauryl cinnamic acid ester and four (2,4- di-tert-butyl-phenyl) 4,4'- biphenylene bisphosphates.
The present invention can match effect, concerted reaction with other raw materials, be avoided that by using the antioxidant of mentioned kind
Transparent PET material at high temperature because minor amount of water there are due to occur hydrolyze and degrade, effectively reduce transparent PET material thermal degradation
Degree and oxidative degradation degree have preferable antioxygenic property, extend service life.More preferably, the antioxidant
For 2,6-di-tert-butyl p-cresol, β-(3,5 di-tert-butyl-hydroxy phenyl) propionic acid octadecyls and thiodipropionic acid dilauryl osmanthus
Acid esters is with weight ratio for 1:2.4-3.2：1.0-1.5 the mixture of composition.
Such as a kind of preparation method of the transparent PET material of high fire-retardance of claim 1-8 any one of them, including walk as follows
Suddenly：
PET resin, nucleating agent, compatilizer and coupling agent are subjected to first time mixing according to parts by weight, then added again
Enter remaining raw material, carries out second and be mixed, obtain mixture；Mixture input extrusion equipment is kneaded, is squeezed out,
It is granulated, the transparent PET material of high fire-retardance is made.
The preparation method of the present invention is simple, convenient operation and control, stable quality, and production efficiency is high, and production cost is low, is suitble to
Large-scale industrial production, transparent PET material obtained have preferable transparency, anti-flammability, heat resistance, smoke-suppressing, stabilization
Property, performances, the processing performance such as anti-oxidant aging it is good, surface is transparent glossy, can help in real time understand by tubing electricity in pipe
The case where line cable, practicability is high, can meet the needs of electric power protection material.
Preferably, the speed of agitator that the first time is mixed is 500-850r/min, second of mixing
Speed of agitator be 900-1100r/min；One area's temperature of the extrusion equipment is 270-280 DEG C, and two area's temperature are 280-285
DEG C, three area's temperature are 285-300 DEG C, and four area's temperature are 295-305 DEG C, and five area's temperature are 270-285 DEG C.
The present invention is by strictly controlling the rotating speed of raw material being mixed twice and each area's temperature of extruding pelletization, energy
Make transparent PET material obtained that there are the power such as preferable transparency, anti-flammability, heat resistance, impact resistance, tensile strength, hardness
Performance is learned, and processability is good, excellent processing performance meets the needs of electric power protection material.
The beneficial effects of the present invention are：The transparent PET material of the present invention has preferable transparency, anti-flammability, heat-resisting
Property, the performances such as smoke-suppressing, stability, anti-oxidant aging, intensity is high, and processability is good, and processing performance is good；Wherein, by using
Fire retardant mutually acts synergistically with synergist, flame retardant effect not only can be improved, but also can play smoke suppressing effect；By using 2,2 '-methylenes
Bis- (4,6- t-butyl phenol) the phosphine aluminium salts of base, dibenzal sorbitol and two (benzal is replaced to chlorine) sorbierites as heat-resistant filler,
And the mixed proportion of three is strictly controlled, crystalline rate can be accelerated, increase crystal density and promote fine grain size, shortened
Molding cycle improves the transparency, tensile strength, rigidity, heat distortion temperature, impact resistance, the creep resistance etc. of transparent PET material
Physical mechanical property, lustrous surface, the case where can help to understand electric wire in pipe in real time by tubing, practicability is high.
The PET material preparation method convenient operation and control of the present invention, stable quality, production efficiency is high, and production cost is low, energy
Make MPP tubing obtained that there are the performances such as preferable transparency, anti-flammability, heat resistance, smoke-suppressing, stability, anti-oxidant aging,
It is suitble to large-scale industrial production.
Specific implementation mode
For the ease of the understanding of those skilled in the art, with reference to embodiment, the present invention is further illustrated, real
The content that the mode of applying refers to not is limitation of the invention.
Embodiment 1
A kind of transparent PET material of high fire-retardance, the transparent PET material include the raw material of following parts by weight：
The nucleating agent is (right by 2,2 '-di-2-ethylhexylphosphine oxides (4,6- t-butyl phenol) phosphine aluminium salt, dibenzal sorbitol and two
Chlorine replace benzal) sorbierite with weight ratio be 2.5:1.2:The mixture of 0.8 composition.
The compatilizer is haloflex.
The fire retardant is three (2,3- dibromopropyl) fulminuric acid esters.
The synergist is antimony oxide.
The coupling agent is vinyltriethoxysilane.
The transparent PET material further includes 1 part of heat-resistant agent, and the heat-resistant agent is magnesium silicide.
The transparent PET material further includes 0.5 part of lubricant, and the lubricant is three hydroxy stearic acid ester of glycerine.
The transparent PET material further includes 2.4 parts of antioxidant, and the antioxidant is 1,3,5- tri- (3,5 tertiary butyl -4- hydroxyls
Base benzyl) trimethylbenzene.
A kind of preparation method of the transparent PET material of high fire-retardance as described above, includes the following steps：
PET resin, nucleating agent, compatilizer and coupling agent are subjected to first time mixing according to parts by weight, then added again
Enter remaining raw material, carries out second and be mixed, obtain mixture；Mixture input extrusion equipment is kneaded, is squeezed out,
It is granulated, the transparent PET material of high fire-retardance is made.
The speed of agitator that the first time is mixed is 500r/min, and the speed of agitator of second of mixing is
900r/min；One area's temperature of the extrusion equipment is 270 DEG C, and two area's temperature are 280 DEG C, and three area's temperature are 285 DEG C, four area's temperature
Degree is 295 DEG C, and five area's temperature are 270 DEG C.
Embodiment 2
A kind of transparent PET material of high fire-retardance, the transparent PET material include the raw material of following parts by weight：
The nucleating agent is (right by 2,2 '-di-2-ethylhexylphosphine oxides (4,6- t-butyl phenol) phosphine aluminium salt, dibenzal sorbitol and two
Chlorine replace benzal) sorbierite with weight ratio be 2.8:1.3:The mixture of 0.9 composition.
The compatilizer is Methylacrylate-Acrylate Copolymer.
The fire retardant is tribromphenol and/or aluminium triphosphate.
The synergist is zinc stannate and/or zinc molybdate.
The coupling agent is anilinomethyl triethoxysilane.
The transparent PET material further includes 2 parts of heat-resistant agents, and the heat-resistant agent is ceramic fibre.
The transparent PET material further includes 1 part of lubricant, and the lubricant is n-butyl stearate.
The transparent PET material further includes 2.6 parts of antioxidant, and the antioxidant is 2,6-di-tert-butyl p-cresol.
A kind of preparation method of the transparent PET material of high fire-retardance as described above, includes the following steps：
PET resin, nucleating agent, compatilizer and coupling agent are subjected to first time mixing according to parts by weight, then added again
Enter remaining raw material, carries out second and be mixed, obtain mixture；Mixture input extrusion equipment is kneaded, is squeezed out,
It is granulated, the transparent PET material of high fire-retardance is made.
The speed of agitator that the first time is mixed is 585r/min, and the speed of agitator of second of mixing is
950r/min；One area's temperature of the extrusion equipment is 272 DEG C, and two area's temperature are 281 DEG C, and three area's temperature are 288 DEG C, four area's temperature
Degree is 298 DEG C, and five area's temperature are 273 DEG C.
Embodiment 3
A kind of transparent PET material of high fire-retardance, the transparent PET material include the raw material of following parts by weight：
The nucleating agent is (right by 2,2 '-di-2-ethylhexylphosphine oxides (4,6- t-butyl phenol) phosphine aluminium salt, dibenzal sorbitol and two
Chlorine replace benzal) sorbierite with weight ratio be 3:1.5:The mixture of 1.0 compositions.
The compatilizer is that natural gum is grafted polymethyl methacrylate and/or styrene-grafted maleic anhydride.
The fire retardant is tetrabromophthalic anhydride and/or eight bromo ether.
The synergist is magnesium silicate and/or zinc borate.
The coupling agent is γ-methacryloxypropyl trimethoxy silane and/or (the 'beta '-methoxy second of vinyl three
Oxygroup) silane.
The transparent PET material further includes 3 parts of heat-resistant agents, and the heat-resistant agent is lignocellulosic.
The transparent PET material further includes 1.5 parts of lubricants, and the lubricant is N, N ,-ethylenebisstearamide and/
Or oleamide.
The transparent PET material further includes 2.8 parts of antioxidant, and the antioxidant is β-(3,5 di-t-butyl -4- hydroxy benzenes
Base) propionic acid octadecyl and/or thiodipropionic acid dilauryl cinnamic acid ester.
A kind of preparation method of the transparent PET material of high fire-retardance as described above, includes the following steps：
PET resin, nucleating agent, compatilizer and coupling agent are subjected to first time mixing according to parts by weight, then added again
Enter remaining raw material, carries out second and be mixed, obtain mixture；Mixture input extrusion equipment is kneaded, is squeezed out,
It is granulated, the transparent PET material of high fire-retardance is made.
The speed of agitator that the first time is mixed is 680r/min, and the speed of agitator of second of mixing is
1000r/min；One area's temperature of the extrusion equipment is 275 DEG C, and two area's temperature are 282 DEG C, and three area's temperature are 292 DEG C, 4th area
Temperature is 300 DEG C, and five area's temperature are 278 DEG C.
Embodiment 4
A kind of transparent PET material of high fire-retardance, the transparent PET material include the raw material of following parts by weight：
The nucleating agent is (right by 2,2 '-di-2-ethylhexylphosphine oxides (4,6- t-butyl phenol) phosphine aluminium salt, dibenzal sorbitol and two
Chlorine replace benzal) sorbierite with weight ratio be 3.2:1.6:The mixture of 1.1 compositions.
The compatilizer is ethylene-acrylic acid-butyl ester graft glycidyl methacrylate.
The fire retardant is dimethyl methyl phosphonate.
The synergist is zinc oxide.
The coupling agent is methyltriethoxysilane.
The transparent PET material further includes 4 parts of heat-resistant agents, and the heat-resistant agent is gas-phase silica.
The transparent PET material further includes 2 parts of lubricants, and the lubricant is that ethylene bis stearamide and/or oxidation are poly-
Ethylene waxes.
The transparent PET material further includes 3 parts of antioxidant, and the antioxidant is 1,3,5- tri- (3,5 di-t-butyl -4- hydroxyls
Base phenyl) isocyanates and/or three (2,4- di-tert-butyl-phenyl) phosphite esters.
A kind of preparation method of the transparent PET material of high fire-retardance as described above, includes the following steps：
PET resin, nucleating agent, compatilizer and coupling agent are subjected to first time mixing according to parts by weight, then added again
Enter remaining raw material, carries out second and be mixed, obtain mixture；Mixture input extrusion equipment is kneaded, is squeezed out,
It is granulated, the transparent PET material of high fire-retardance is made.
The speed of agitator that the first time is mixed is 775r/min, and the speed of agitator of second of mixing is
1050r/min；One area's temperature of the extrusion equipment is 278 DEG C, and two area's temperature are 283 DEG C, and three area's temperature are 296 DEG C, 4th area
Temperature is 302 DEG C, and five area's temperature are 282 DEG C.
Embodiment 5
A kind of transparent PET material of high fire-retardance, the transparent PET material include the raw material of following parts by weight：
The nucleating agent is (right by 2,2 '-di-2-ethylhexylphosphine oxides (4,6- t-butyl phenol) phosphine aluminium salt, dibenzal sorbitol and two
Chlorine replace benzal) sorbierite with weight ratio be 3.5:1.8:The mixture of 1.2 compositions.
The compatilizer is penylene dimaleimide.
The fire retardant is that tetrabromobisphenol A is bis- (2,3- dibromopropyl ether).
The synergist is zinc borate.
The coupling agent is pyrophosphate titanate esters.
The transparent PET material further includes 5 parts of heat-resistant agents, and the heat-resistant agent is wollastonite in powder.
The transparent PET material further includes 2.5 parts of lubricants, and the lubricant is zinc stearate and/or stearmide.
The transparent PET material further includes 3.2 parts of antioxidant, and the antioxidant is four (2,4- di-tert-butyl-phenyls) 4,
4'- biphenylene bisphosphates.
A kind of preparation method of the transparent PET material of high fire-retardance as described above, includes the following steps：
PET resin, nucleating agent, compatilizer and coupling agent are subjected to first time mixing according to parts by weight, then added again
Enter remaining raw material, carries out second and be mixed, obtain mixture；Mixture input extrusion equipment is kneaded, is squeezed out,
It is granulated, the transparent PET material of high fire-retardance is made.
The speed of agitator that the first time is mixed is 850r/min, and the speed of agitator of second of mixing is
1100r/min；One area's temperature of the extrusion equipment is 280 DEG C, and two area's temperature are 285 DEG C, and three area's temperature are 300 DEG C, 4th area
Temperature is 305 DEG C, and five area's temperature are 285 DEG C.
Embodiment 6
The present embodiment and embodiment 1 difference lies in：
The compatilizer is to be grafted polymethyl methacrylate by Methylacrylate-Acrylate Copolymer, natural gum
With penylene dimaleimide with weight ratio for 1.6：2.5:The mixture of 1 composition.
The fire retardant is by three (2,3- dibromopropyl) fulminuric acid esters, dimethyl methyl phosphonate and tetrabromo-phthalic two
Formic anhydride is with weight ratio for 1.2:1:The mixture of 2.5 compositions.
The synergist is with weight ratio by zinc stannate, zinc molybdate, magnesium silicate and zinc borate for 0.8:1：1.5：2.4 composition
Mixture.
The coupling agent is γ-methacryloxypropyl trimethoxy silane, methyltriethoxysilane and ethylene
('beta '-methoxy ethyoxyl) silane of base three is with weight ratio for 2.5:1:The mixture of 1.4 compositions.
It with weight ratio is 1 that the heat-resistant agent, which is ceramic fibre, magnesium silicide and lignocellulosic,:1.2:The mixing of 2.5 compositions
Object.
The lubricant is N, N, and-ethylenebisstearamide, stearmide and oxidized polyethylene wax are with weight ratio
0.8:1：The mixture of 2.4 compositions.
The antioxidant is 2,6-di-tert-butyl p-cresol, β-(3,5 di-tert-butyl-hydroxy phenyl) propionic acid octadecyl
With thiodipropionic acid dilauryl cinnamic acid ester with weight ratio for 1:2.4：The mixture of 1.0 compositions.
Embodiment 7
The present embodiment the difference from example 2 is that：
The compatilizer is to be grafted polymethyl methacrylate by Methylacrylate-Acrylate Copolymer, natural gum
With penylene dimaleimide with weight ratio for 1.8：2.8:The mixture of 1 composition.
The fire retardant is by three (2,3- dibromopropyl) fulminuric acid esters, dimethyl methyl phosphonate and tetrabromo-phthalic two
Formic anhydride is with weight ratio for 1.3:1:The mixture of 2.8 compositions.
The synergist is with weight ratio by zinc stannate, zinc molybdate, magnesium silicate and zinc borate for 0.9:1：1.3：2.6 composition
Mixture.
The coupling agent is γ-methacryloxypropyl trimethoxy silane, methyltriethoxysilane and ethylene
('beta '-methoxy ethyoxyl) silane of base three is with weight ratio for 2.8:1:The mixture of 1.6 compositions.
It with weight ratio is 1 that the heat-resistant agent, which is ceramic fibre, magnesium silicide and lignocellulosic,:1.3:The mixing of 2.8 compositions
Object.
The lubricant is N, N, and-ethylenebisstearamide, stearmide and oxidized polyethylene wax are with weight ratio
0.9:1：The mixture of 2.6 compositions.
The antioxidant is 2,6-di-tert-butyl p-cresol, β-(3,5 di-tert-butyl-hydroxy phenyl) propionic acid octadecyl
With thiodipropionic acid dilauryl cinnamic acid ester with weight ratio for 1:2.6：The mixture of 1.1 compositions.
Embodiment 8
The present embodiment and embodiment 3 difference lies in：
The compatilizer is to be grafted polymethyl methacrylate by Methylacrylate-Acrylate Copolymer, natural gum
With penylene dimaleimide with weight ratio for 2：3:The mixture of 1 composition.
The fire retardant is by three (2,3- dibromopropyl) fulminuric acid esters, dimethyl methyl phosphonate and tetrabromo-phthalic two
Formic anhydride is with weight ratio for 1.5:1:The mixture of 3 compositions.
The synergist is with weight ratio by zinc stannate, zinc molybdate, magnesium silicate and zinc borate for 1:1：1.2：2.8 compositions
Mixture.
The coupling agent is γ-methacryloxypropyl trimethoxy silane, methyltriethoxysilane and ethylene
('beta '-methoxy ethyoxyl) silane of base three is with weight ratio for 3:1:The mixture of 1.8 compositions.
It with weight ratio is 1 that the heat-resistant agent, which is ceramic fibre, magnesium silicide and lignocellulosic,:1.5:The mixture of 3 compositions.
The lubricant is N, N, and-ethylenebisstearamide, stearmide and oxidized polyethylene wax are with weight ratio for 1:
1：The mixture of 2.8 compositions.
The antioxidant is 2,6-di-tert-butyl p-cresol, β-(3,5 di-tert-butyl-hydroxy phenyl) propionic acid octadecyl
With thiodipropionic acid dilauryl cinnamic acid ester with weight ratio for 1:2.8：1.2 the mixture of composition.
Embodiment 9
The present embodiment and embodiment 4 difference lies in：
The compatilizer is to be grafted polymethyl methacrylate by Methylacrylate-Acrylate Copolymer, natural gum
With penylene dimaleimide with weight ratio for 2.2：3.2:The mixture of 1 composition.
The fire retardant is by three (2,3- dibromopropyl) fulminuric acid esters, dimethyl methyl phosphonate and tetrabromo-phthalic two
Formic anhydride is with weight ratio for 1.6:1:3.2 the mixture of composition.
The synergist is with weight ratio by zinc stannate, zinc molybdate, magnesium silicate and zinc borate for 1.1:1：1.1：3 compositions
Mixture.
The coupling agent is γ-methacryloxypropyl trimethoxy silane, methyltriethoxysilane and ethylene
('beta '-methoxy ethyoxyl) silane of base three is with weight ratio for 3.2:1:The mixture of 2 compositions.
It with weight ratio is 1 that the heat-resistant agent, which is ceramic fibre, magnesium silicide and lignocellulosic,:1.6:The mixing of 3.2 compositions
Object.
The lubricant is N, N, and-ethylenebisstearamide, stearmide and oxidized polyethylene wax are with weight ratio
1.1:1：The mixture of 3 compositions.
The antioxidant is 2,6-di-tert-butyl p-cresol, β-(3,5 di-tert-butyl-hydroxy phenyl) propionic acid octadecyl
With thiodipropionic acid dilauryl cinnamic acid ester with weight ratio for 1:3：The mixture of 1.3 compositions.
Embodiment 10
The present embodiment and embodiment 5 difference lies in：
The compatilizer is to be grafted polymethyl methacrylate by Methylacrylate-Acrylate Copolymer, natural gum
With penylene dimaleimide with weight ratio for 2.4：3.5:The mixture of 1 composition.
The fire retardant is by three (2,3- dibromopropyl) fulminuric acid esters, dimethyl methyl phosphonate and tetrabromo-phthalic two
Formic anhydride is with weight ratio for 1.8:1:The mixture of 3.5 compositions.
The synergist is with weight ratio by zinc stannate, zinc molybdate, magnesium silicate and zinc borate for 1.2:1：1.0：3.2 composition
Mixture.
The coupling agent is γ-methacryloxypropyl trimethoxy silane, methyltriethoxysilane and ethylene
('beta '-methoxy ethyoxyl) silane of base three is with weight ratio for 3.5:1:The mixture of 2.2 compositions.
It with weight ratio is 1 that the heat-resistant agent, which is ceramic fibre, magnesium silicide and lignocellulosic,:1.8:The mixing of 3.5 compositions
Object.
The lubricant is N, N, and-ethylenebisstearamide, stearmide and oxidized polyethylene wax are with weight ratio
1.2:1：The mixture of 3.2 compositions.
The antioxidant is 2,6-di-tert-butyl p-cresol, β-(3,5 di-tert-butyl-hydroxy phenyl) propionic acid octadecyl
With thiodipropionic acid dilauryl cinnamic acid ester with weight ratio for 1:3.2：The mixture of 1.5 compositions.
Comparative example 1
A kind of PET material of high fire-retardance, the PET material include the raw material of following parts by weight：
The compatilizer is that natural gum is grafted polymethyl methacrylate and/or styrene-grafted maleic anhydride.
The fire retardant is tetrabromophthalic anhydride and/or eight bromo ether.
The synergist is magnesium silicate and/or zinc borate.
The coupling agent is γ-methacryloxypropyl trimethoxy silane and/or (the 'beta '-methoxy second of vinyl three
Oxygroup) silane.
The PET material further includes 3 parts of heat-resistant agents, and the heat-resistant agent is lignocellulosic.
The PET material further includes 1.5 parts of lubricants, and the lubricant is N, N ,-ethylenebisstearamide and/or oil
Sour amide.
The PET material further includes 2.8 parts of antioxidant, and the antioxidant is β-(3,5 di-tert-butyl-hydroxy phenyl) third
Sour octadecyl and/or thiodipropionic acid dilauryl cinnamic acid ester.
A kind of preparation method of the PET material of high fire-retardance as described above, includes the following steps：
PET resin, compatilizer and coupling agent are subjected to first time mixing according to parts by weight, then added remaining
Raw material carries out second and is mixed, obtains mixture；Mixture input extrusion equipment is kneaded, squeezed out, is granulated, is made
Obtain the PET material of high fire-retardance.
The speed of agitator that the first time is mixed is 680r/min, and the speed of agitator of second of mixing is
1000r/min；One area's temperature of the extrusion equipment is 275 DEG C, and two area's temperature are 282 DEG C, and three area's temperature are 292 DEG C, 4th area
Temperature is 300 DEG C, and five area's temperature are 278 DEG C.
Comparative example 2
A kind of transparent PET material, the transparent PET material include the raw material of following parts by weight：
The nucleating agent is (right by 2,2 '-di-2-ethylhexylphosphine oxides (4,6- t-butyl phenol) phosphine aluminium salt, dibenzal sorbitol and two
Chlorine replace benzal) sorbierite with weight ratio be 3:1.5:The mixture of 1.0 compositions.
The compatilizer is that natural gum is grafted polymethyl methacrylate and/or styrene-grafted maleic anhydride.
The coupling agent is γ-methacryloxypropyl trimethoxy silane and/or (the 'beta '-methoxy second of vinyl three
Oxygroup) silane.
The transparent PET material further includes 3 parts of heat-resistant agents, and the heat-resistant agent is lignocellulosic.
The transparent PET material further includes 1.5 parts of lubricants, and the lubricant is N, N ,-ethylenebisstearamide and/
Or oleamide.
The transparent PET material further includes 2.8 parts of antioxidant, and the antioxidant is β-(3,5 di-t-butyl -4- hydroxy benzenes
Base) propionic acid octadecyl and/or thiodipropionic acid dilauryl cinnamic acid ester.
A kind of preparation method of transparent PET material as described above, includes the following steps：
PET resin, nucleating agent, compatilizer and coupling agent are subjected to first time mixing according to parts by weight, then added again
Enter remaining raw material, carries out second and be mixed, obtain mixture；Mixture input extrusion equipment is kneaded, is squeezed out,
It is granulated, transparent PET material is made.
The speed of agitator that the first time is mixed is 680r/min, and the speed of agitator of second of mixing is
1000r/min；One area's temperature of the extrusion equipment is 275 DEG C, and two area's temperature are 282 DEG C, and three area's temperature are 292 DEG C, 4th area
Temperature is 300 DEG C, and five area's temperature are 278 DEG C.
Finished product made from above-described embodiment 1-10 and comparative example 1-2 is subjected to the performance tests such as fire protecting performance respectively, is tested
As a result as follows：
By upper table data it is found that the transparent PET material of the present invention has preferable transparency, anti-flammability, heat resistance, suppression cigarette
Property, the performances such as stability, anti-oxidant aging, intensity is high, and processability is good, and processing performance is good；Wherein, implementation through the invention
Example 1-10 and comparative example 1-2 compares, and the present invention mutually acts synergistically by using fire retardant with synergist, and fire-retardant effect both can be improved
Fruit, and smoke suppressing effect can be played；By using 2,2 '-di-2-ethylhexylphosphine oxides (4,6- t-butyl phenol) phosphine aluminium salt, dibenzal sorbitol
With two (replacing benzal to chlorine) sorbierites, as heat-resistant filler, crystalline rate can be accelerated, increase crystal density and promote crystal grain ruler
Molding cycle, the transparency of raising transparent PET material, tensile strength, rigidity, heat distortion temperature, shock resistance are shortened in very little miniaturization
Property, the physical mechanical properties such as creep resistance, lustrous surface can help to the feelings for understanding electric wire in pipe in real time by tubing
Condition, practicability is high, meets the needs of electric power protection material.
Above-described embodiment is the preferable implementation of the present invention, and in addition to this, the present invention can be realized with other manner,
Any obvious replacement is not departed under the premise of present inventive concept within protection scope of the present invention.
Claims (10)
1. a kind of transparent PET material of high fire-retardance, it is characterised in that：The transparent PET material includes the raw material of following parts by weight：
The nucleating agent (is taken to chlorine by 2,2 '-di-2-ethylhexylphosphine oxides (4,6- t-butyl phenol) phosphine aluminium salt, dibenzal sorbitol and two
For benzal) sorbierite with weight ratio is 2.5-3.5:1.2-1.8:The mixture of 0.8-1.2 compositions.
2. a kind of transparent PET material of high fire-retardance according to claim 1, it is characterised in that：The compatilizer is chlorination
Polyethylene, Methylacrylate-Acrylate Copolymer, penylene dimaleimide, natural gum are grafted poly-methyl methacrylate
At least one of ester, styrene-grafted maleic anhydride and ethylene-acrylic acid-butyl ester graft glycidyl methacrylate.
3. a kind of transparent PET material of high fire-retardance according to claim 1, it is characterised in that：The fire retardant be three (2,
3- dibromopropyls) fulminuric acid ester, tribromphenol, aluminium triphosphate, dimethyl methyl phosphonate, tetrabromobisphenol A bis- (2,3- bis-
Bromopropyl ether), at least one of tetrabromophthalic anhydride and eight bromo ether.
4. a kind of transparent PET material of high fire-retardance according to claim 1, it is characterised in that：The synergist is three oxygen
Change at least one of two antimony, zinc stannate, zinc molybdate, magnesium silicate, zinc borate, zinc oxide and zinc borate.
5. a kind of transparent PET material of high fire-retardance according to claim 1, it is characterised in that：The coupling agent is ethylene
Ethyl triethoxy silicane alkane, anilinomethyl triethoxysilane, γ-methacryloxypropyl trimethoxy silane, methyl three
At least one of Ethoxysilane, pyrophosphate titanate esters and vinyl three ('beta '-methoxy ethyoxyl) silane.
6. a kind of transparent PET material of high fire-retardance according to claim 1, it is characterised in that：The transparent PET material is also
Including 1-5 parts of heat-resistant agents, the heat-resistant agent is in magnesium silicide, ceramic fibre, lignocellulosic, gas-phase silica and wollastonite in powder
At least one.
7. a kind of transparent PET material of high fire-retardance according to claim 1, it is characterised in that：The transparent PET material is also
Including 0.5-2.5 parts of lubricants, the lubricant is N, N ,-ethylenebisstearamide, oleamide, n-butyl stearate,
At least one of three hydroxy stearic acid ester of glycerine, ethylene bis stearamide, stearmide, zinc stearate and oxidized polyethylene wax.
8. a kind of transparent PET material of high fire-retardance according to claim 1, it is characterised in that：The transparent PET material is also
Including 2.4-3.2 parts of antioxidant, the antioxidant is 2,6-di-tert-butyl p-cresol, 1,3,5- tri- (3,5 tertiary butyl-4-hydroxies
Benzyl) trimethylbenzene, β-(3,5 di-tert-butyl-hydroxy phenyl) propionic acid octadecyl, 1,3,5- tri- (3,5 di-t-butyl -4-
Hydroxy phenyl) isocyanates, three (2,4- di-tert-butyl-phenyl) phosphite esters, thiodipropionic acid dilauryl cinnamic acid ester and four (2,4-
At least one of di-tert-butyl-phenyl) 4,4'- biphenylene bisphosphates.
9. the preparation method of the transparent PET material such as a kind of high fire-retardance of claim 1-8 any one of them, it is characterised in that：
Include the following steps：
PET resin, nucleating agent, compatilizer and coupling agent are subjected to first time mixing according to parts by weight, then added surplus
Remaining raw material carries out second and is mixed, obtains mixture；Mixture input extrusion equipment is kneaded, squeezed out, is made
The transparent PET material of high fire-retardance is made in grain.
10. a kind of preparation method of the transparent PET material of high fire-retardance according to claim 9, it is characterised in that：Described
The speed of agitator of mixed once stirring is 500-850r/min, and described second speed of agitator being mixed is 900-1100r/
min；One area's temperature of the extrusion equipment is 270-280 DEG C, and two area's temperature are 280-285 DEG C, and three area's temperature are 285-300
DEG C, four area's temperature are 295-305 DEG C, and five area's temperature are 270-285 DEG C.
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Cited By (3)
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| CN110157162A (en) * | 2019-06-08 | 2019-08-23 | 纳琳威纳米科技南通有限公司 | Stiffened anti-flaming thermal-insulation master batch and its manufacturing method |
| CN112961471A (en) * | 2019-11-28 | 2021-06-15 | 湖南尚鑫新材料科技有限公司 | High-heat-sealing high-light-transmittance glass film and preparation method thereof |
| CN114921067A (en) * | 2022-05-23 | 2022-08-19 | 东莞市锦源高分子科技有限公司 | PET (polyethylene terephthalate) high-transparency smooth master batch and production process thereof |
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| US20100240814A1 (en) * | 2007-12-24 | 2010-09-23 | Cheil Industries Inc. | Flame-Retardant Polyester Resin Composition Having Excellent Heat Resistance |
| CN102504500A (en) * | 2011-10-26 | 2012-06-20 | 惠州市沃特新材料有限公司 | PET (polyethylene terephthalate) engineering plastic and preparation method and application thereof |
| CN103113725A (en) * | 2013-03-22 | 2013-05-22 | 上海顶新箱包有限公司 | PET (Polyethylene Terephthalate) resin composition as well as preparation method and application thereof |
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| US20100240814A1 (en) * | 2007-12-24 | 2010-09-23 | Cheil Industries Inc. | Flame-Retardant Polyester Resin Composition Having Excellent Heat Resistance |
| CN102504500A (en) * | 2011-10-26 | 2012-06-20 | 惠州市沃特新材料有限公司 | PET (polyethylene terephthalate) engineering plastic and preparation method and application thereof |
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| CN110157162A (en) * | 2019-06-08 | 2019-08-23 | 纳琳威纳米科技南通有限公司 | Stiffened anti-flaming thermal-insulation master batch and its manufacturing method |
| CN112961471A (en) * | 2019-11-28 | 2021-06-15 | 湖南尚鑫新材料科技有限公司 | High-heat-sealing high-light-transmittance glass film and preparation method thereof |
| CN114921067A (en) * | 2022-05-23 | 2022-08-19 | 东莞市锦源高分子科技有限公司 | PET (polyethylene terephthalate) high-transparency smooth master batch and production process thereof |
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