CN104559077A - Nano modified PBT (polybutylece terephthalate) resin and preparation method thereof - Google Patents

Nano modified PBT (polybutylece terephthalate) resin and preparation method thereof Download PDF

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Publication number
CN104559077A
CN104559077A CN201410275422.XA CN201410275422A CN104559077A CN 104559077 A CN104559077 A CN 104559077A CN 201410275422 A CN201410275422 A CN 201410275422A CN 104559077 A CN104559077 A CN 104559077A
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temperature
district
butyl
compound
ester
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郑豪
胡正宏
王强
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DONGGUAN YIHAO NANO COMPOSITES SCIENCE AND TECHNOL
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郑豪
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Abstract

The invention discloses nano modified PBT (polybutylece terephthalate) resin and a preparation method thereof. The nano modified PBT resin comprises the following components in percentage by weight: 40-60% of PBT polyester, 20-40% of glass fibers, 0.4% of a lubricant, 0.6% of an antioxidant, 1% of a toughening agent, 13% of a flame retardant, 4% of a synergistic flame retardant and 1% of a nano nucleating agent. By virtue of the material proportion, the nano modified PBT resin has the advantages of good toughness, good mechanical properties and good fireproof performance, and the toughness, the wear resistance, the high-temperature resistance and the aging resistance are greatly improved, so that the nano modified PBT resin can well meet operating requirements and operating environments. Besides, the preparation method comprises the steps of weighing materials, mixing and stirring, and performing extrusion granulation by using a double-screw extruder. By virtue of the design of the process steps, the preparation method of the nano modified PBT resin, disclosed by the invention, is simple in process and low in cost.

Description

A kind of nano modification PBT resin and preparation method thereof
Technical field
The present invention relates to plastic material technical field, particularly relate to a kind of nano modification PBT resin and preparation method thereof.
Background technology
Polybutylene terephthalate resin (polybutylene terephthalate, be called for short PBT), formed by 1.4-pbt butyleneglycol (1.4-Butylene glycol) and terephthalic acid (PTA) or terephthalate (DMT) polycondensation, and the oyster white made via mixing program is translucent to opaque, crystalline thermoplastic polyester's resin, thermoplastic polyester is referred to as together with PET, or saturated polyester.
PBT has excellent physical and mechanical properties in wide temperature range, and life-time service temperature can reach 120 DEG C, and electrical insulating property is excellent, and even under high-temperature high-frequency, its electrical property is still better, and creep resistance, resistance to fatigue, rub resistance, dimensional stability are all fine.
But for existing PBT resin, it is poor that it still exists flame retardant resistance, be HB rank, poor toughness, shock strength is low, the oxygen generation crosslinking reaction in melting process easily and in air, and make viscosity unstable, the second-order transition temperature of amorphous phase is lower.
Summary of the invention
The object of the invention is to provide a kind of nano modification PBT resin for the deficiencies in the prior art, this nano modification PBT resin good toughness, mechanical property is good and fire resistance is good, toughness, wear-resisting, high temperature resistant and anti-aging aspect are greatly improved, and namely can meet service requirements and environment for use well.
Another object of the present invention is to provide a kind of nano modification PBT resin preparation method, this nano modification PBT resin preparation method technique is simple, with low cost.
For achieving the above object, the present invention is achieved through the following technical solutions.
A kind of nano modification PBT resin, includes the material of following weight ratio, is specially:
PBT polyester 40%-60%
Glass fibre 20%-40%
Lubricant 0.4%
Antioxidant 0.6%
Toughner 1 %
Fire retardant 13%
Synergistic flame retardant 4%
Nano-nucleating agent 1%;
Wherein, lubricant is montanic acid, sodium stearate, the compound that refining wax forms or pentaerythritol stearate or ethylene bis-fatty acid amides, antioxidant is 1, 3, 5-tri-(the 4-tertiary butyl-3-alkyl-2, 6-3,5-dimethylphenyl)-1, 3, 5-triazine-2, 4, 6-(1H, 3H, the compound that 5H)-triketone and Tyox B form or N, N '-hexa-methylene two (3, 5-di-t-butyl-4-alkyl hydrocinnamamide) and tricresyl phosphite (2, 4-di-tert-butyl-phenyl) compound that forms of ester or spiral shell butyleneglycol two [2, 2 '-methylene-bis (4, 6-di-tert-butyl-phenyl)] phosphorous acid ester and four [2, 4-di-tert-butyl-phenyl-4, 4 '-xenyl] compound that forms of biphosphonate or four [methyl-β-(3, 5-di-tert-butyl-hydroxy phenyl) propionic ester] pentaerythritol ester and phosphorous acid ester three (2, 4-di-tert-butyl-phenyl) compound that forms of ester, toughner is selected from epoxy group(ing) for having, amino, the compound of more than one groups in isocyanate group, fire retardant is brominated epoxy, brominated polyphenylene or TDE, synergistic flame retardant is antimonous oxide, sodium antimonate, sodium antimoniate, anhydrous sodium antimonate or anhydrous sodium antimoniate.
Further, a kind of nano modification PBT resin, includes the material of following weight ratio, is specially:
PBT polyester 50%
Glass fibre 30%
Lubricant 0.4%
Antioxidant 0.6%
Toughner 1%
Fire retardant 13%
Synergistic flame retardant 4%
Nano-nucleating agent 1%;
Wherein, lubricant is montanic acid, sodium stearate, the compound that refining wax forms or pentaerythritol stearate or ethylene bis-fatty acid amides, antioxidant is 1, 3, 5-tri-(the 4-tertiary butyl-3-alkyl-2, 6-3,5-dimethylphenyl)-1, 3, 5-triazine-2, 4, 6-(1H, 3H, the compound that 5H)-triketone and Tyox B form or N, N '-hexa-methylene two (3, 5-di-t-butyl-4-alkyl hydrocinnamamide) and tricresyl phosphite (2, 4-di-tert-butyl-phenyl) compound that forms of ester or spiral shell butyleneglycol two [2, 2 '-methylene-bis (4, 6-di-tert-butyl-phenyl)] phosphorous acid ester and four [2, 4-di-tert-butyl-phenyl-4, 4 '-xenyl] compound that forms of biphosphonate or four [methyl-β-(3, 5-di-tert-butyl-hydroxy phenyl) propionic ester] pentaerythritol ester and phosphorous acid ester three (2, 4-di-tert-butyl-phenyl) compound that forms of ester, toughner is selected from epoxy group(ing) for having, amino, the compound of more than one groups in isocyanate group, fire retardant is brominated epoxy, brominated polyphenylene or TDE, synergistic flame retardant is antimonous oxide, sodium antimonate, sodium antimoniate, anhydrous sodium antimonate or anhydrous sodium antimoniate.
A kind of nano modification PBT resin preparation method, includes following processing step, is specially:
A, take material according to weight ratio;
B, PBT polyester, glass fibre, lubricant, antioxidant, toughner, fire retardant, synergistic flame retardant, nano-nucleating agent are poured in mixing tank and carry out stirring at normal temperature mixing, stirring velocity is 960r/min, and churning time is 2-3 minute;
C, mixed material is placed in twin screw extruder and complete melting successively, extrude, granulation, wherein, twin screw one district temperature is 220-240 DEG C, two district's temperature are for being 230-260 DEG C, three district's temperature are 230-260 DEG C, four district's temperature are 230-260 DEG C, five district's temperature are 225-255 DEG C, six district's temperature are 225-255 DEG C, and seven district's temperature are 220-250 DEG C, and eight district's temperature are 220-250 DEG C, nine district's temperature are 220-250 DEG C, head temperature is 230-260 DEG C, and the residence time of material in barrel is 1-2 minute, and melt pressure is 10-30MPa.
Further, a kind of nano modification PBT resin preparation method, includes following processing step, is specially:
A, take material according to weight ratio;
B, PBT polyester, glass fibre, lubricant, antioxidant, toughner, fire retardant, synergistic flame retardant, nano-nucleating agent are poured in mixing tank and carry out stirring at normal temperature mixing, stirring velocity is 960r/min, and churning time is 2-3 minute;
C, mixed material is placed in twin screw extruder and complete melting successively, extrude, granulation, wherein, twin screw one district temperature is 220 DEG C, two district's temperature are for being 250 DEG C, and three district's temperature are 250 DEG C, and four district's temperature are 245 DEG C, five district's temperature are 240 DEG C, six district's temperature are 235 DEG C, and seven district's temperature are 230 DEG C, and eight district's temperature are 230 DEG C, nine district's temperature are 230 DEG C, head temperature is 245 DEG C, and the residence time of material in barrel is 1-2 minute, and melt pressure is 10-30MPa.
Beneficial effect of the present invention is: a kind of nano modification PBT resin of the present invention, and it comprises PBT polyester 40%-60%, glass fibre 20%-40%, lubricant 0.4%, antioxidant 0.6%, toughner 1%, fire retardant 13%, synergistic flame retardant 4%, nano-nucleating agent 1%; Nano-nucleating agent can increase toughness, and glass fibre can improve mechanical property, and add fire retardant and can improve multiple fire resistance, glass fibre is through coupling agent treatment and unclassified stores is macromolecular material, and this makes there is good consistency between all materials; So nano modification PBT resin of the present invention has the good and advantage that fire resistance is good of good toughness, mechanical property, and toughness, wear-resisting, high temperature resistant and anti-aging aspect are greatly improved, and namely can meet service requirements and environment for use well.
Another beneficial effect of the present invention is: a kind of nano modification PBT resin preparation method of the present invention, and it comprises material and takes step, mix and blend step, twin screw extruder extruding pelletization step; Designed by above-mentioned processing step, nano modification PBT resin preparation method technique of the present invention is simple and with low cost.
Embodiment
Below in conjunction with concrete embodiment, the present invention will be described.
Embodiment one, a kind of nano modification PBT resin, includes the material of following weight ratio, is specially:
PBT polyester 50%
Glass fibre 30%
Lubricant 0.4%
Antioxidant 0.6%
Toughner 1%
Fire retardant 13%
Synergistic flame retardant 4%
Nano-nucleating agent 1%;
Wherein, lubricant is pentaerythritol stearate, antioxidant is four [methyl-β-(3, 5-di-tert-butyl-hydroxy phenyl) propionic ester] pentaerythritol ester and phosphorous acid ester three (2, 4-di-tert-butyl-phenyl) compound that forms of ester, four [methyl-β-(3 in antioxidant, 5-di-tert-butyl-hydroxy phenyl) propionic ester] pentaerythritol ester and phosphorous acid ester three (2, 4-di-tert-butyl-phenyl) weight ratio of ester is 1:1, i.e. four [methyl-β-(3 in antioxidant, 5-di-tert-butyl-hydroxy phenyl) propionic ester] pentaerythritol ester and phosphorous acid ester three (2, 4-di-tert-butyl-phenyl) ester accounts for the weight ratio 0.3% of total material respectively, toughner is ethylene-methyl methacrylate glycidyl ester copolymer, and fire retardant is brominated Polystyrene, and synergistic flame retardant is antimonous oxide.
Need to explain further, the compound that the lubricant of the present embodiment one can also form for montanic acid, sodium stearate, refining wax or ethylene bis-fatty acid amides, namely the lubricant of the present embodiment one can be montanic acid, sodium stearate, a kind of or two or more the formed blend refined in compound that wax form, pentaerythritol stearate, ethylene bis-fatty acid amides.
In addition, the antioxidant of the present embodiment one can also be 1, 3, 5-tri-(the 4-tertiary butyl-3-alkyl-2, 6-3,5-dimethylphenyl)-1, 3, 5-triazine-2, 4, 6-(1H, 3H, the compound that 5H)-triketone and Tyox B form or N, N '-hexa-methylene two (3, 5-di-t-butyl-4-alkyl hydrocinnamamide) and tricresyl phosphite (2, 4-di-tert-butyl-phenyl) compound that forms of ester or spiral shell butyleneglycol two [2, 2 '-methylene-bis (4, 6-di-tert-butyl-phenyl)] phosphorous acid ester and four [2, 4-di-tert-butyl-phenyl-4, 4 '-xenyl] compound that forms of biphosphonate, the i.e. antioxidant of the present embodiment one blend that can form for above-mentioned a kind of compound or two or more compound, two kinds of weight of material contained by above-mentioned various compound are than being 1:1.
The toughner of the present embodiment one is selected from epoxy group(ing) for having, amino, the compound of more than one groups in isocyanate group, namely toughner can be bisphenol A type epoxy resin, novolac epoxy, 3-isocyanate group propyl-triethoxysilicane or olefines grafts, such as POE-G-GMA, POE-G-MAH, SEBS-G-GMA, SEBS-G-MAH, SBS-MAH, EPDM-G-GMA, EPDM-g-MAH, EPDM-g-St, ethylene-methyl methacrylate glycidyl ester copolymer; Wherein, the toughner of the present embodiment one blend that can form for above-mentioned a kind of toughner or more than two kinds toughner.
The brominated Polystyrene of the present embodiment one is the one in brominated polyphenylene, and certainly, the fire retardant of the present embodiment one can also be brominated epoxy or TDE; Wherein, the fire retardant of the present embodiment one blend that can form for a kind of or two or more fire retardant in above-mentioned fire retardant.The synergistic flame retardant of the present embodiment one is Sb system fire retardant, and the present embodiment one, except antimonous oxide can be adopted as except synergistic flame retardant, can also adopt anhydrous sodium antimoniate, sodium antimonate, sodium antimoniate or anhydrous sodium antimonate as synergistic flame retardant; Wherein, the synergistic flame retardant of the present embodiment one blend that can form for above-mentioned a kind of Sb system fire retardant or two or more Sb system fire retardant.
Need point out further, the trade mark that the PBT polyester of the present embodiment one can be produced for Yizheng, Jiangsu petrochemical complex limited-liability company is the PBT polyester of XW321; the glass fibre of the present embodiment one for the trade mark that Taishan glass fiber Ltd produces be the glass fibre of ERS-T635B, the pentaerythritol stearate of the present embodiment one for the trade mark that Italian Fa Ji company produces be the pentaerythritol stearate of PETS-AP, four [methyl-β-(3 of the present embodiment one, 5-di-tert-butyl-hydroxy phenyl) propionic ester] pentaerythritol ester for the trade mark that Albemarle Corporation of the U.S. produces be four [methyl-β-(3 of AT-10,5-di-tert-butyl-hydroxy phenyl) propionic ester] pentaerythritol ester, the phosphorous acid ester three (2 of the present embodiment one, 4-di-tert-butyl-phenyl) ester for the trade mark that Albemarle Corporation of the U.S. produces be the phosphorous acid ester three (2 of AT-168,4-di-tert-butyl-phenyl) ester, the ethylene-methyl methacrylate glycidyl ester copolymer of the present embodiment one for the trade mark that French Arkema produces be the ethylene-methyl methacrylate glycidyl ester copolymer of AX-8900, the brominated Polystyrene of the present embodiment one for the trade mark that Albemarle Corporation of the U.S. produces be the brominated Polystyrene of 621, the antimonous oxide of the present embodiment one is the antimonous oxide of the Hunan China mattress trade mark, the nano-nucleating agent of the present embodiment one for the trade mark that Jiangsu nine river scientific & technical corporation produces be the nano-nucleating agent of TW03.
Need point out further, by above-mentioned material proportion, nano-nucleating agent can increase the toughness of PBT resin, and glass fibre can improve the mechanical property of PBT resin, adds the fire resistance that fire retardant can improve PBT resin; Wherein, glass fibre is through coupling agent treatment, and unclassified stores is macromolecular material, and this makes there is good consistency between all materials, and toughness, the aspect such as wear-resisting, high temperature resistant, anti-aging have greatly improved, and can meet its service requirements and environment for use.
 
Embodiment two, a kind of nano modification PBT resin, includes the material of following weight ratio, is specially:
PBT polyester 60%
Glass fibre 20%
Lubricant 0.4%
Antioxidant 0.6%
Toughner 1%
Fire retardant 13%
Synergistic flame retardant 4%
Nano-nucleating agent 1%;
Wherein, lubricant is pentaerythritol stearate, antioxidant is four [methyl-β-(3, 5-di-tert-butyl-hydroxy phenyl) propionic ester] pentaerythritol ester and phosphorous acid ester three (2, 4-di-tert-butyl-phenyl) compound that forms of ester, four [methyl-β-(3 in antioxidant, 5-di-tert-butyl-hydroxy phenyl) propionic ester] pentaerythritol ester and phosphorous acid ester three (2, 4-di-tert-butyl-phenyl) weight ratio of ester is 1:1, i.e. four [methyl-β-(3 in antioxidant, 5-di-tert-butyl-hydroxy phenyl) propionic ester] pentaerythritol ester and phosphorous acid ester three (2, 4-di-tert-butyl-phenyl) ester accounts for the weight ratio 0.3% of total material respectively, toughner is ethylene-methyl methacrylate glycidyl ester copolymer, and fire retardant is brominated Polystyrene, and synergistic flame retardant is antimonous oxide.
Need to explain further, the compound that the lubricant of the present embodiment two can also form for montanic acid, sodium stearate, refining wax or ethylene bis-fatty acid amides, namely the lubricant of the present embodiment two can be montanic acid, sodium stearate, a kind of or two or more the formed blend refined in compound that wax form, pentaerythritol stearate, ethylene bis-fatty acid amides.
In addition, the antioxidant of the present embodiment two can also be 1, 3, 5-tri-(the 4-tertiary butyl-3-alkyl-2, 6-3,5-dimethylphenyl)-1, 3, 5-triazine-2, 4, 6-(1H, 3H, the compound that 5H)-triketone and Tyox B form or N, N '-hexa-methylene two (3, 5-di-t-butyl-4-alkyl hydrocinnamamide) and tricresyl phosphite (2, 4-di-tert-butyl-phenyl) compound that forms of ester or spiral shell butyleneglycol two [2, 2 '-methylene-bis (4, 6-di-tert-butyl-phenyl)] phosphorous acid ester and four [2, 4-di-tert-butyl-phenyl-4, 4 '-xenyl] compound that forms of biphosphonate, the i.e. antioxidant of the present embodiment two blend that can form for above-mentioned a kind of compound or two or more compound, two kinds of weight of material contained by above-mentioned various compound are than being 1:1.
The toughner of the present embodiment two is selected from epoxy group(ing) for having, amino, the compound of more than one groups in isocyanate group, namely toughner can be bisphenol A type epoxy resin, novolac epoxy, 3-isocyanate group propyl-triethoxysilicane or olefines grafts, such as POE-G-GMA, POE-G-MAH, SEBS-G-GMA, SEBS-G-MAH, SBS-MAH, EPDM-G-GMA, EPDM-g-MAH, EPDM-g-St, ethylene-methyl methacrylate glycidyl ester copolymer; Wherein, the toughner of the present embodiment two blend that can form for above-mentioned a kind of toughner or more than two kinds toughner.
The brominated Polystyrene of the present embodiment two is the one in brominated polyphenylene, and certainly, the fire retardant of the present embodiment two can also be brominated epoxy or TDE; Wherein, the fire retardant of the present embodiment two blend that can form for a kind of or two or more fire retardant in above-mentioned fire retardant.The synergistic flame retardant of the present embodiment two is Sb system fire retardant, and the present embodiment two, except antimonous oxide can be adopted as except synergistic flame retardant, can also adopt anhydrous sodium antimoniate, sodium antimonate, sodium antimoniate or anhydrous sodium antimonate as synergistic flame retardant; Wherein, the synergistic flame retardant of the present embodiment two blend that can form for above-mentioned a kind of Sb system fire retardant or two or more Sb system fire retardant.
Need point out further, the trade mark that the PBT polyester of the present embodiment two can be produced for Yizheng, Jiangsu petrochemical complex limited-liability company is the PBT polyester of XW321; the glass fibre of the present embodiment two for the trade mark that Taishan glass fiber Ltd produces be the glass fibre of ERS-T635B, the pentaerythritol stearate of the present embodiment two for the trade mark that Italian Fa Ji company produces be the pentaerythritol stearate of PETS-AP, four [methyl-β-(3 of the present embodiment two, 5-di-tert-butyl-hydroxy phenyl) propionic ester] pentaerythritol ester for the trade mark that Albemarle Corporation of the U.S. produces be four [methyl-β-(3 of AT-10,5-di-tert-butyl-hydroxy phenyl) propionic ester] pentaerythritol ester, the phosphorous acid ester three (2 of the present embodiment two, 4-di-tert-butyl-phenyl) ester for the trade mark that Albemarle Corporation of the U.S. produces be the phosphorous acid ester three (2 of AT-168,4-di-tert-butyl-phenyl) ester, the ethylene-methyl methacrylate glycidyl ester copolymer of the present embodiment two for the trade mark that French Arkema produces be the ethylene-methyl methacrylate glycidyl ester copolymer of AX-8900, the brominated Polystyrene of the present embodiment two for the trade mark that Albemarle Corporation of the U.S. produces be the brominated Polystyrene of 621, the antimonous oxide of the present embodiment two is the antimonous oxide of the Hunan China mattress trade mark, the nano-nucleating agent of the present embodiment two for the trade mark that Jiangsu nine river scientific & technical corporation produces be the nano-nucleating agent of TW03.
Need point out further, by above-mentioned material proportion, nano-nucleating agent can increase the toughness of PBT resin, and glass fibre can improve the mechanical property of PBT resin, adds the fire resistance that fire retardant can improve PBT resin; Wherein, glass fibre is through coupling agent treatment, and unclassified stores is macromolecular material, and this makes there is good consistency between all materials, and toughness, the aspect such as wear-resisting, high temperature resistant, anti-aging have greatly improved, and can meet its service requirements and environment for use.
 
Embodiment three, a kind of nano modification PBT resin, includes the material of following weight ratio, is specially:
PBT polyester 40%
Glass fibre 40%
Lubricant 0.4%
Antioxidant 0.6%
Toughner 1%
Fire retardant 13%
Synergistic flame retardant 4%
Nano-nucleating agent 1%;
Wherein, lubricant is pentaerythritol stearate, antioxidant is four [methyl-β-(3, 5-di-tert-butyl-hydroxy phenyl) propionic ester] pentaerythritol ester and phosphorous acid ester three (2, 4-di-tert-butyl-phenyl) compound that forms of ester, four [methyl-β-(3 in antioxidant, 5-di-tert-butyl-hydroxy phenyl) propionic ester] pentaerythritol ester and phosphorous acid ester three (2, 4-di-tert-butyl-phenyl) weight ratio of ester is 1:1, i.e. four [methyl-β-(3 in antioxidant, 5-di-tert-butyl-hydroxy phenyl) propionic ester] pentaerythritol ester and phosphorous acid ester three (2, 4-di-tert-butyl-phenyl) ester accounts for the weight ratio 0.3% of total material respectively, toughner is ethylene-methyl methacrylate glycidyl ester copolymer, and fire retardant is brominated Polystyrene, and synergistic flame retardant is antimonous oxide.
Need to explain further, the compound that the lubricant of the present embodiment three can also form for montanic acid, sodium stearate, refining wax or ethylene bis-fatty acid amides, namely the lubricant of the present embodiment three can be montanic acid, sodium stearate, a kind of or two or more the formed blend refined in compound that wax form, pentaerythritol stearate, ethylene bis-fatty acid amides.
In addition, the antioxidant of the present embodiment three can also be 1, 3, 5-tri-(the 4-tertiary butyl-3-alkyl-2, 6-3,5-dimethylphenyl)-1, 3, 5-triazine-2, 4, 6-(1H, 3H, the compound that 5H)-triketone and Tyox B form or N, N '-hexa-methylene two (3, 5-di-t-butyl-4-alkyl hydrocinnamamide) and tricresyl phosphite (2, 4-di-tert-butyl-phenyl) compound that forms of ester or spiral shell butyleneglycol two [2, 2 '-methylene-bis (4, 6-di-tert-butyl-phenyl)] phosphorous acid ester and four [2, 4-di-tert-butyl-phenyl-4, 4 '-xenyl] compound that forms of biphosphonate, the i.e. antioxidant of the present embodiment three blend that can form for above-mentioned a kind of compound or two or more compound, two kinds of weight of material contained by above-mentioned various compound are than being 1:1.
The toughner of the present embodiment three is selected from epoxy group(ing) for having, amino, the compound of more than one groups in isocyanate group, namely toughner can be bisphenol A type epoxy resin, novolac epoxy, 3-isocyanate group propyl-triethoxysilicane or olefines grafts, such as POE-G-GMA, POE-G-MAH, SEBS-G-GMA, SEBS-G-MAH, SBS-MAH, EPDM-G-GMA, EPDM-g-MAH, EPDM-g-St, ethylene-methyl methacrylate glycidyl ester copolymer; Wherein, the toughner of the present embodiment three blend that can form for above-mentioned a kind of toughner or more than two kinds toughner.
The brominated Polystyrene of the present embodiment three is the one in brominated polyphenylene, and certainly, the fire retardant of the present embodiment three can also be brominated epoxy or TDE; Wherein, the fire retardant of the present embodiment three blend that can form for a kind of or two or more fire retardant in above-mentioned fire retardant.The synergistic flame retardant of the present embodiment three is Sb system fire retardant, and the present embodiment three, except antimonous oxide can be adopted as except synergistic flame retardant, can also adopt anhydrous sodium antimoniate, sodium antimonate, sodium antimoniate or anhydrous sodium antimonate as synergistic flame retardant; Wherein, the synergistic flame retardant of the present embodiment three blend that can form for above-mentioned a kind of Sb system fire retardant or two or more Sb system fire retardant.
Need point out further, the trade mark that the PBT polyester of the present embodiment three can be produced for Yizheng, Jiangsu petrochemical complex limited-liability company is the PBT polyester of XW321; the glass fibre of the present embodiment three for the trade mark that Taishan glass fiber Ltd produces be the glass fibre of ERS-T635B, the pentaerythritol stearate of the present embodiment three for the trade mark that Italian Fa Ji company produces be the pentaerythritol stearate of PETS-AP, four [methyl-β-(3 of the present embodiment three, 5-di-tert-butyl-hydroxy phenyl) propionic ester] pentaerythritol ester for the trade mark that Albemarle Corporation of the U.S. produces be four [methyl-β-(3 of AT-10,5-di-tert-butyl-hydroxy phenyl) propionic ester] pentaerythritol ester, the phosphorous acid ester three (2 of the present embodiment three, 4-di-tert-butyl-phenyl) ester for the trade mark that Albemarle Corporation of the U.S. produces be the phosphorous acid ester three (2 of AT-168,4-di-tert-butyl-phenyl) ester, the ethylene-methyl methacrylate glycidyl ester copolymer of the present embodiment three for the trade mark that French Arkema produces be the ethylene-methyl methacrylate glycidyl ester copolymer of AX-8900, the brominated Polystyrene of the present embodiment three for the trade mark that Albemarle Corporation of the U.S. produces be the brominated Polystyrene of 621, the antimonous oxide of the present embodiment three is the antimonous oxide of the Hunan China mattress trade mark, the nano-nucleating agent of the present embodiment three for the trade mark that Jiangsu nine river scientific & technical corporation produces be the nano-nucleating agent of TW03.
Need point out further, by above-mentioned material proportion, nano-nucleating agent can increase the toughness of PBT resin, and glass fibre can improve the mechanical property of PBT resin, adds the fire resistance that fire retardant can improve PBT resin; Wherein, glass fibre is through coupling agent treatment, and unclassified stores is macromolecular material, and this makes there is good consistency between all materials, and toughness, the aspect such as wear-resisting, high temperature resistant, anti-aging have greatly improved, and can meet its service requirements and environment for use.
 
Embodiment four, a kind of nano modification PBT resin preparation method, includes following processing step, is specially:
A, take material according to above-mentioned weight ratio;
B, PBT polyester, glass fibre, lubricant, antioxidant, toughner, fire retardant, synergistic flame retardant, nano-nucleating agent are poured in mixing tank and carry out stirring at normal temperature mixing, stirring velocity is 960r/min, and churning time is 2-3 minute;
C, mixed material is placed in twin screw extruder and complete melting successively, extrude, granulation, wherein, twin screw one district temperature is 220 DEG C, two district's temperature are for being 250 DEG C, and three district's temperature are 250 DEG C, and four district's temperature are 245 DEG C, five district's temperature are 240 DEG C, six district's temperature are 235 DEG C, and seven district's temperature are 230 DEG C, and eight district's temperature are 230 DEG C, nine district's temperature are 230 DEG C, head temperature is 245 DEG C, and the residence time of material in barrel is 1-2 minute, and melt pressure is 10-30MPa.
Above content is only preferred embodiment of the present invention, and for those of ordinary skill in the art, according to thought of the present invention, all will change in specific embodiments and applications, this description should not be construed as limitation of the present invention.

Claims (4)

1. a nano modification PBT resin, is characterized in that, includes the material of following weight ratio, is specially:
PBT polyester 40%-60%
Glass fibre 20%-40%
Lubricant 0.4%
Antioxidant 0.6%
Toughner 1%
Fire retardant 13%
Synergistic flame retardant 4%
Nano-nucleating agent 1%;
Wherein, lubricant is montanic acid, sodium stearate, the compound that refining wax forms or pentaerythritol stearate or ethylene bis-fatty acid amides, antioxidant is 1, 3, 5-tri-(the 4-tertiary butyl-3-alkyl-2, 6-3,5-dimethylphenyl)-1, 3, 5-triazine-2, 4, 6-(1H, 3H, the compound that 5H)-triketone and Tyox B form or N, N '-hexa-methylene two (3, 5-di-t-butyl-4-alkyl hydrocinnamamide) and tricresyl phosphite (2, 4-di-tert-butyl-phenyl) compound that forms of ester or spiral shell butyleneglycol two [2, 2 '-methylene-bis (4, 6-di-tert-butyl-phenyl)] phosphorous acid ester and four [2, 4-di-tert-butyl-phenyl-4, 4 '-xenyl] compound that forms of biphosphonate or four [methyl-β-(3, 5-di-tert-butyl-hydroxy phenyl) propionic ester] pentaerythritol ester and phosphorous acid ester three (2, 4-di-tert-butyl-phenyl) compound that forms of ester, toughner is selected from epoxy group(ing) for having, amino, the compound of more than one groups in isocyanate group, fire retardant is brominated epoxy, brominated polyphenylene or TDE, synergistic flame retardant is antimonous oxide, sodium antimonate, sodium antimoniate, anhydrous sodium antimonate or anhydrous sodium antimoniate.
2. a kind of nano modification PBT resin according to claim 1, is characterized in that, include the material of following weight ratio, be specially:
PBT polyester 50%
Glass fibre 30%
Lubricant 0.4%
Antioxidant 0.6%
Toughner 1%
Fire retardant 13%
Synergistic flame retardant 4%
Nano-nucleating agent 1%;
Wherein, lubricant is montanic acid, sodium stearate, the compound that refining wax forms or pentaerythritol stearate or ethylene bis-fatty acid amides, antioxidant is 1, 3, 5-tri-(the 4-tertiary butyl-3-alkyl-2, 6-3,5-dimethylphenyl)-1, 3, 5-triazine-2, 4, 6-(1H, 3H, the compound that 5H)-triketone and Tyox B form or N, N '-hexa-methylene two (3, 5-di-t-butyl-4-alkyl hydrocinnamamide) and tricresyl phosphite (2, 4-di-tert-butyl-phenyl) compound that forms of ester or spiral shell butyleneglycol two [2, 2 '-methylene-bis (4, 6-di-tert-butyl-phenyl)] phosphorous acid ester and four [2, 4-di-tert-butyl-phenyl-4, 4 '-xenyl] compound that forms of biphosphonate or four [methyl-β-(3, 5-di-tert-butyl-hydroxy phenyl) propionic ester] pentaerythritol ester and phosphorous acid ester three (2, 4-di-tert-butyl-phenyl) compound that forms of ester, toughner is selected from epoxy group(ing) for having, amino, the compound of more than one groups in isocyanate group, fire retardant is brominated epoxy, brominated polyphenylene or TDE, synergistic flame retardant is antimonous oxide, sodium antimonate, sodium antimoniate, anhydrous sodium antimonate or anhydrous sodium antimoniate.
3. a nano modification PBT resin preparation method, this nano modification PBT resin is the nano modification PBT resin described in claims 1 or 2, it is characterized in that, includes following processing step, be specially:
A, take material according to weight ratio;
B, PBT polyester, glass fibre, lubricant, antioxidant, toughner, fire retardant, synergistic flame retardant, nano-nucleating agent are poured in mixing tank and carry out stirring at normal temperature mixing, stirring velocity is 960r/min, and churning time is 2-3 minute;
C, mixed material is placed in twin screw extruder and complete melting successively, extrude, granulation, wherein, twin screw one district temperature is 220-240 DEG C, two district's temperature are for being 230-260 DEG C, three district's temperature are 230-260 DEG C, four district's temperature are 230-260 DEG C, five district's temperature are 225-255 DEG C, six district's temperature are 225-255 DEG C, and seven district's temperature are 220-250 DEG C, and eight district's temperature are 220-250 DEG C, nine district's temperature are 220-250 DEG C, head temperature is 230-260 DEG C, and the residence time of material in barrel is 1-2 minute, and melt pressure is 10-30MPa.
4. a kind of nano modification PBT resin preparation method according to claim 4, is characterized in that, include following processing step, be specially:
A, take material according to weight ratio;
B, PBT polyester, glass fibre, lubricant, antioxidant, toughner, fire retardant, synergistic flame retardant, nano-nucleating agent are poured in mixing tank and carry out stirring at normal temperature mixing, stirring velocity is 960r/min, and churning time is 2-3 minute;
C, mixed material is placed in twin screw extruder and complete melting successively, extrude, granulation, wherein, twin screw one district temperature is 220 DEG C, two district's temperature are for being 250 DEG C, and three district's temperature are 250 DEG C, and four district's temperature are 245 DEG C, five district's temperature are 240 DEG C, six district's temperature are 235 DEG C, and seven district's temperature are 230 DEG C, and eight district's temperature are 230 DEG C, nine district's temperature are 230 DEG C, head temperature is 245 DEG C, and the residence time of material in barrel is 1-2 minute, and melt pressure is 10-30MPa.
CN201410275422.XA 2014-06-20 2014-06-20 Nano modified PBT (polybutylece terephthalate) resin and preparation method thereof Pending CN104559077A (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101613480A (en) * 2009-07-30 2009-12-30 上海金发科技发展有限公司 A kind of preparation method who strengthens the polybutylene terephthalate flame-retardant heat conduction material
CN103059525A (en) * 2013-01-18 2013-04-24 江门市奇德工程塑料科技有限公司 High-temperature-resisting xanthochroia-resisting high-performance flame retarding PET (Polyethylene Terephthalate) composite material and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101613480A (en) * 2009-07-30 2009-12-30 上海金发科技发展有限公司 A kind of preparation method who strengthens the polybutylene terephthalate flame-retardant heat conduction material
CN103059525A (en) * 2013-01-18 2013-04-24 江门市奇德工程塑料科技有限公司 High-temperature-resisting xanthochroia-resisting high-performance flame retarding PET (Polyethylene Terephthalate) composite material and preparation method thereof

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