CN102321347A - High creepage trace index polyester composite and preparation method thereof - Google Patents
High creepage trace index polyester composite and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of high creepage trace index polyester composite and preparation method thereof.High creepage trace index polyester composite, composed of the following components by weight percentage: saturated polyester 40～60%; Composite flame-retardant agent 8～18%; Toughner 2～5%; Thermo-stabilizer 0.3～1%; Spun glass 20～40%; Described saturated polyester material is polybutylene terephthalate and/or polyethylene terephthalate; Described composite flame-retardant agent comprises main flame retardant agent and auxiliary flame retardant, and described main flame retardant agent is brominated flame retardant and/or P-N type fire retardant, and auxiliary flame retardant is that two or more MOX is composite.Not only electric property is good for high creepage trace index polyester composite of the present invention, and need not add nucleator and nucleation accelerating agent, so cost is comparatively cheap.
Description
Technical field
The invention belongs to technical field of polymer materials, relate to a kind of high creepage trace index polyester composite and preparation method thereof, this material can be widely used in field of electronics, field of household appliances.
Background technology
Polybutylene terephthalate (PBT) and polyethylene terephthalate (PET) are daily common thermoplastic polyester plastic, and be cheap and easy to get.Its defective is that notched Izod impact strength is low, and molding shrinkage is big, easy firing, so major part adopts fire retardant, spun glass to strengthen or be inorganic filling-modified, its tensile strength, flexural strength can be enhanced about more than once, and heat-drawn wire significantly improves.Germany BASF, Bayer, U.S. GE, Ticona, Japanese Toray, Mitsubishi Chemical, companies such as the new photosynthetic fibre in Taiwan, Changchun artificial resin, South Asia plastics all have very sophisticated product on market, to circulate.It is fast that the product of these companies all has crystallization velocity, and the most suitable forming method is injection moulding.
Some is easy to generate electrical spark with the appliance material that PBT processes when switching on, mainly be that the defective of PBT itself causes.Polyester electricity trace reaction mechanism and polyester pyrolysis mechanism have similarity, are enough to make polyester generation thermolysis by the heat of discharge generation.The thermotolerance of PET is higher than PBT, thereby PBT is than the easier electric traceization of PET.The PET material that on market, circulates is generally expensive than PBT material, is because the crystallization velocity of PET is very slow, must add nucleator and nucleation accelerating agent, just has use value.
Summary of the invention
The technical problem that the present invention will solve is, provides a kind of and need not add nucleator and nucleation accelerating agent, and cost is lower, and the good high creepage trace index polyester composite of electric property.
The technical problem that the present invention further will solve is, the preparation method of simple, the easy to operate above-mentioned high creepage trace polyester composite of a kind of technology is provided.
In order to solve the problems of the technologies described above, the technical scheme that the present invention adopts is, a kind of high creepage trace index polyester composite is composed of the following components by weight percentage:
Saturated polyester 40～60%;
Composite flame-retardant agent 8～18%;
Toughner 2～5%;
Thermo-stabilizer 0.3～1%;
Spun glass 20～40%;
Described saturated polyester material is polybutylene terephthalate and/or polyethylene terephthalate; Described composite flame-retardant agent comprises main flame retardant agent and auxiliary flame retardant, and described main flame retardant agent is brominated flame retardant and/or P-N type fire retardant, and auxiliary flame retardant is that two or more MOX is composite.
The limiting viscosity of said polybutylene terephthalate is 0.7-1.2, and the limiting viscosity of said polyethylene terephthalate is 0.65-1.1.
Described brominated flame retardant is a TDE, and the P-N type fire retardant is a polyphosphoric acid melamine; Described compound auxilliary fire retardant comprises Antimony Trioxide: 99.5Min and zinc borate.
Described toughner is self-control toughner, and main ingredient is methyl acrylate glycidyl ester, maleic anhydride graft terpolymer EP rubber.
Described self-control toughner by weight percentage; Use twin screw extruder to do grafting equipment with methyl acrylate glycidyl ester 1.5%, maleic anhydride 0.5% and terpolymer EP rubber 98%, extrusion temperature is methyl acrylate glycidyl ester, the maleic anhydride graft terpolymer EP rubber that 170 degree obtain.
Described thermo-stabilizer comprises four [methyl-β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic ester] pentaerythritol ester and three [2.4-di-tert-butyl-phenyl] phosphorous acid ester.
The diameter of described spun glass is 3～5 microns.
Above-described high creepage trace index polyester composite, by weight percentage can be composed of the following components:
Polybutylene terephthalate 36～41%;
Polyethylene terephthalate 10～14%;
TDE 8～11%;
Polyphosphoric acid melamine 1～3%;
Antimony Trioxide: 99.5Min 1～3%;
Zinc borate 1～3%;
Toughner 3～5%;
Thermo-stabilizer 0.3～1%;
Spun glass 25～35%.
A kind of preparing method's of above-mentioned high creepage trace index polyester composite technical scheme may further comprise the steps:
(1) takes by weighing saturated polyester, toughner, thermo-stabilizer, composite flame-retardant agent, spun glass successively;
(2) saturated polyester, toughner, thermo-stabilizer, composite flame-retardant agent middling speed are mixed;
(3) with raw material mixed in the step (2) and spun glass blending, melt extrude granulation through twin screw extruder.
Above-described preparation method can also may further comprise the steps:
In step (2), saturated polyester, composite flame-retardant agent, toughner, thermo-stabilizer middling speed were mixed 3-7 minute;
The twin screw extruder processing condition are in step (3): twin screw extruder one district's temperature is 210～260 ℃; Two district's temperature are 210～260 ℃; Three district's temperature are 210～260 ℃; Four district's temperature are 210～260 ℃, 210～260 ℃ in five districts, and compound time of delivery in screw rod is 0.5～1 minute.
Not only electric property is good for high creepage trace index polyester composite of the present invention, and need not add nucleator and nucleation accelerating agent, so cost is comparatively cheap.
Embodiment
Below in conjunction with embodiment the present invention is done detailed explanation:
PBT selects sticking L2100 in the Yizheng Fiber Optical plant of Jiangsu, and PET selects Jiangsu San Fangxiang to produce low sticking CZ5011;
Toughner is homemade methyl acrylate glycidyl ester, maleic anhydride graft terpolymer EP rubber (GMA-MAH-g-EPDM); Selected terpolymer EP rubber is that Du Pont produces 4725P, and methyl acrylate glycidyl ester (GMA) is commercially available, and maleic anhydride (MAH) is that Shanghai medicine group produces the analytical pure level; Use twin screw extruder to do grafting equipment; By weight percentage, GMA uses 1.5%, and MAH uses 0.5%; 4725P uses 98%, and extrusion temperature is 170 degree.
Brominated flame retardant in the main flame retardant produces ten monobromethanes for Shouguang, Shandong, and P-N type fire-retartant agent MP P (polyphosphoric acid melamine) uses MPP not reach the effect of fire-retardant V0 separately for Hangzhou Jie Ersi produces.
Antimony Trioxide: 99.5Min in the auxilliary fire retardant produces for the Dongguan Jeff, and zinc borate is that safe star chemical industry produces.
Spun glass is that tai shan glass group produces, and the diameter of spun glass is 3～5 microns, and the trade mark is T635B
Thermo-stabilizer is that Beijing addition additive factory produces.
Embodiment 1, with PBT L2100 weight percent (down with) 56.6%, and thermo-stabilizer (1010 and 168) respectively 0.2%; Self-control toughner (GMA-MAH-g-EPDM) 3%, compound main flame retardant TDE 5%, MPP 1%; Compound auxiliary flame retardant Antimony Trioxide: 99.5Min 2%, zinc borate 2% was middling speed stirrer for mixing 5 minutes; With 30% glass blending, be that 210--260 ℃ of twin screw extruder extruded granulation again through melt temperature.Wherein each zone temperatures is: 210 ℃ in a district, and 250 ℃ in two districts, 255 ℃ in three districts, 260 ℃ in four districts, 245 ℃ in five districts, the residence time was 50 seconds.
Embodiment 2, and with PBT L2100 weight percent (down with) 49.6%, PET CZ50011 is 5%, thermo-stabilizer (1010 and 168) respectively 0.2%; Self-control toughner (GMA-MAH-g-EPDM) 3%, compound main flame retardant TDE 7%, MPP 1%; Compound auxiliary flame retardant Antimony Trioxide: 99.5Min 2%, zinc borate 2% was middling speed stirrer for mixing 5 minutes; With 30% glass blending, be that 210--260 ℃ of twin screw extruder extruded granulation again through melt temperature.Wherein each zone temperatures is: 210 ℃ in a district, and 250 ℃ in two districts, 255 ℃ in three districts, 260 ℃ in four districts, 245 ℃ in five districts, the residence time was 50 seconds.
Embodiment 3, and with PBT L2100 weight percent (down with) 45.6%, PET CZ50011 is 7%, thermo-stabilizer (1010 and 168) respectively 0.2%; Self-control toughner (GMA-MAH-g-EPDM) 3%, compound main flame retardant TDE 8%, MPP 2%; Compound auxiliary flame retardant Antimony Trioxide: 99.5Min 2%, zinc borate 2% was middling speed stirrer for mixing 5 minutes; With 30% glass blending, be that 210--260 ℃ of twin screw extruder extruded granulation again through melt temperature.Wherein each zone temperatures is: 210 ℃ in a district, and 250 ℃ in two districts, 255 ℃ in three districts, 260 ℃ in four districts, 245 ℃ in five districts, the residence time was 50 seconds.
Embodiment 4, and with PBT L2100 weight percent (down with) 40.6%, PET CZ50011 is 12%, thermo-stabilizer (1010 and 168) respectively 0.2%; Self-control toughner (GMA-MAH-g-EPDM) 3%, compound main flame retardant TDE 10%, MPP 2%; Compound auxiliary flame retardant Antimony Trioxide: 99.5Min 2%, zinc borate 2% was middling speed stirrer for mixing 5 minutes; With 30% glass blending, be that 210--260 ℃ of twin screw extruder extruded granulation again through melt temperature.Wherein each zone temperatures is: 210 ℃ in a district, and 250 ℃ in two districts, 255 ℃ in three districts, 260 ℃ in four districts, 245 ℃ in five districts, the residence time was 50 seconds.
Embodiment 5, and with PBT L2100 weight percent (down with) 38.6%, PET CZ50011 is 12%, thermo-stabilizer (1010 and 168) respectively 0.2%; Self-control toughner (GMA-MAH-g-EPDM) 3%, compound main flame retardant TDE 10%, MPP 2%; Compound auxiliary flame retardant Antimony Trioxide: 99.5Min 2%, zinc borate 2% was middling speed stirrer for mixing 5 minutes; With 30% glass blending, be that 210--260 ℃ of twin screw extruder extruded granulation again through melt temperature.Wherein each zone temperatures is: 210 ℃ in a district, and 250 ℃ in two districts, 255 ℃ in three districts, 260 ℃ in four districts, 245 ℃ in five districts, the residence time was 50 seconds.
Embodiment 6, and with PBT L2100 weight percent (down with) 30.6%, PET CZ50011 is 20%, thermo-stabilizer (1010 and 168) respectively 0.2%; Self-control toughner (GMA-MAH-g-EPDM) 3%, compound main flame retardant TDE 10%, MPP 2%; Compound auxiliary flame retardant Antimony Trioxide: 99.5Min 2%, zinc borate 2% was middling speed stirrer for mixing 5 minutes; With 30% glass blending, be that 210--260 ℃ of twin screw extruder extruded granulation again through melt temperature.Wherein each zone temperatures is: 210 ℃ in a district, and 250 ℃ in two districts, 255 ℃ in three districts, 260 ℃ in four districts, 245 ℃ in five districts, the residence time was 50 seconds.
Embodiment 7, and with PBT L2100 weight percent (down together) 40.6%, PET CZ50011 is 12%; Thermo-stabilizer (1010 and 168) each 0.2%, self-control toughner (GMA-MAH-g-EPDM) 3%, compound main flame retardant TDE 10%; Compound auxiliary flame retardant Antimony Trioxide: 99.5Min 2%, zinc borate 2% was middling speed stirrer for mixing 5 minutes; With 30% glass blending, be that 210--260 ℃ of twin screw extruder extruded granulation again through melt temperature.Wherein each zone temperatures is: 210 ℃ in a district, and 250 ℃ in two districts, 255 ℃ in three districts, 260 ℃ in four districts, 245 ℃ in five districts, the residence time was 50 seconds.
Comparative Examples 1, with PBT L2100 weight percent (down together) 40.6%, PET CZ50011 is 12%; Thermo-stabilizer (1010 and 168) each 0.2%, self-control toughner (GMA-MAH-g-EPDM) 3%, MPP is 14%; Middling speed stirrer for mixing 5 minutes; With 30% glass blending, be that 210--260 ℃ of twin screw extruder extruded granulation again through melt temperature.Wherein each zone temperatures is: 210 ℃ in a district, and 250 ℃ in two districts, 255 ℃ in three districts, 260 ℃ in four districts, 245 ℃ in five districts, the residence time was 50 seconds.
Comparative Examples 2, with PBT L2100 weight percent (down together) 39.6%, PET CZ50011 is 12%; Thermo-stabilizer (1010 and 168) each 0.2%, self-control toughner (GMA-MAH-g-EPDM) 3%, compound main flame retardant TDE 10%; MPP is 2%, and auxiliary flame retardant Antimony Trioxide: 99.5Min 3% was middling speed stirrer for mixing 5 minutes; With 30% glass blending, be that 210--260 ℃ of twin screw extruder extruded granulation again through melt temperature.Wherein each zone temperatures is: 210 ℃ in a district, and 250 ℃ in two districts, 255 ℃ in three districts, 260 ℃ in four districts, 245 ℃ in five districts, the residence time was 50 seconds.
Comparative Examples 3, with PBT L2100 weight percent (down together) 38.6%, PET CZ50011 is 12%; Thermo-stabilizer (1010 and 168) each 0.2%, self-control toughner (GMA-MAH-g-EPDM) 3%, compound main flame retardant TDE 10%; MPP is 2%, and auxiliary flame retardant zinc borate 4% was middling speed stirrer for mixing 5 minutes; With 30% glass blending, be that 210--260 ℃ of twin screw extruder extruded granulation again through melt temperature.Wherein each zone temperatures is: 210 ℃ in a district, and 250 ℃ in two districts, 255 ℃ in three districts, 260 ℃ in four districts, 245 ℃ in five districts, the residence time was 50 seconds.
Performance evaluation mode and implementation standard
The particle that above-mentioned 6 embodiment and 4 Comparative Examples are accomplished granulations in 130--150 ℃ convection oven dry 4-6 hour again with the injection moulding sample preparation on the 80T injection moulding machine of exsiccant particle, keeps the mould temperature between 70-100 ℃ in the sample making course.
Tensile strength is tested by GB/T 1040 standards., specimen types is the I type, batten size (mm): 170 (length) * (20 ± 0.2) (end width) * (4 ± 0.2) (thickness), and draw speed is 50mm/min; Flexural strength and modulus in flexure are tested by GB 9341/T standard.Specimen types is specimen size (mm): (80 ± 2) * (10 ± 0.2) * (4 ± 0.2), rate of bending are 20mm/min; Notched Izod impact strength is tested by the GB/T1043 standard.Specimen types is the I type, specimen size (mm): (80 ± 2) * (10 ± 0.2) * (4 ± 0.2); The breach type is a category-A, and the breach residual thickness is 3.2mm; Heat-drawn wire is tested by the GB/T1634.2 standard, and load is 100mm. for the 1.80MPa. span.Flame retardant properties makes an experiment according to the standard of UL94; To be 3.2mm and 1.6mm. creepage trace index make an experiment according to the standard of UL746A batten thickness; Batten thickness is that the 3.23mm. surface gloss makes an experiment according to GB9754-88; Mainly be that with the naked eye to watch spline surfaces, the size of batten be 300mm * 150mm * 20mm
Embodiment 1-6 and Comparative Examples 1-4 raw material weight umber and the composite property table of processing
The creepage trace index of Comparative Examples 1 is the highest, and when halogen-free flame retardants had been used in this explanation, the anti creepage trace performance of material increased substantially, but the but reduction significantly of other performances, and particularly shock strength is low, causes this prescription not have practicality.The creepage trace index of embodiment 6 is 500V, but surface gloss is relatively poor, and this and PET crystallization velocity are slow, are difficult for nucleation, cause surface appearance very poor.Comprehensive other performances, the result optimal of embodiment 5 is different, existing higher creepage trace index, surface appearance is good, and impact, flame retardant properties reach balance.
The crystallization velocity of low sticking PET faster than in sticking and high sticking PET, select saturated polyester composite, be less than or equal at PET content in 15% the scope, can not use nucleator and nucleation accelerating agent, the crystallization velocity of whole formula system and thermotolerance can reach balance.
Claims (10)
1. one kind high creepage trace index polyester composite is characterized in that, and is composed of the following components by weight percentage:
Saturated polyester 40～60%;
Composite flame-retardant agent 8～18%;
Toughner 2～5%;
Thermo-stabilizer 0.3～1%;
Spun glass 20～40%;
Described saturated polyester material is polybutylene terephthalate and/or polyethylene terephthalate; Described composite flame-retardant agent comprises main flame retardant agent and auxiliary flame retardant, and described main flame retardant agent is brominated flame retardant and/or P-N type fire retardant, and auxiliary flame retardant is that two or more MOX is composite.
2. a kind of high creepage trace index polyester composite according to claim 1 is characterized in that the limiting viscosity of said polybutylene terephthalate is 0.7-1.2, and the limiting viscosity of said polyethylene terephthalate is 0.65-1.1.
3. high creepage trace index polyester composite according to claim 1 is characterized in that described brominated flame retardant is a TDE, and the P-N type fire retardant is a polyphosphoric acid melamine; Described compound auxilliary fire retardant comprises Antimony Trioxide: 99.5Min and zinc borate.
4. high creepage trace index polyester composite according to claim 1 is characterized in that, described toughner is self-control toughner, and main ingredient is methyl acrylate glycidyl ester, maleic anhydride graft terpolymer EP rubber.
5. high creepage trace index polyester composite according to claim 4; It is characterized in that; Described self-control toughner by weight percentage; Use twin screw extruder to do grafting equipment with methyl acrylate glycidyl ester 1.5%, maleic anhydride 0.5% and terpolymer EP rubber 98%, extrusion temperature is methyl acrylate glycidyl ester, the maleic anhydride graft terpolymer EP rubber that 170 degree obtain.
6. high creepage trace index polyester composite according to claim 1; It is characterized in that; Described thermo-stabilizer comprises four [methyl-β-(3, the 5-di-tert-butyl-hydroxy phenyl) propionic ester] pentaerythritol ester and three [2.4-di-tert-butyl-phenyl] phosphorous acid ester.
7. high creepage trace index polyester composite according to claim 1 is characterized in that the diameter of described spun glass is 3～5 microns.
8. high creepage trace index polyester composite according to claim 1 is characterized in that, by weight
Per-cent is composed of the following components;
Polybutylene terephthalate 36～41%;
Polyethylene terephthalate 10～14%;
TDE 8～11%;
Polyphosphoric acid melamine 1～3%;
Antimony Trioxide: 99.5Min 1～3%;
Zinc borate 1～3%;
Toughner 3～5%;
Thermo-stabilizer 0.3～1%;
Spun glass 25～35%.
9. the preparation method of the said high creepage trace index polyester composite of arbitrary claim in the claim 1 to 8 is characterized in that, may further comprise the steps:
(1) takes by weighing saturated polyester, toughner, thermo-stabilizer, composite flame-retardant agent, spun glass successively;
(2) saturated polyester, toughner, thermo-stabilizer, composite flame-retardant agent middling speed are mixed;
(3) with raw material mixed in the step (2) and spun glass blending, melt extrude granulation through twin screw extruder.
10. the described preparation method of claim 9 is characterized in that, may further comprise the steps:
In step (2), saturated polyester, composite flame-retardant agent, toughner, thermo-stabilizer middling speed were mixed 3-7 minute;
The twin screw extruder processing condition are in step (3): twin screw extruder one district's temperature is 210～260 ℃; Two district's temperature are 210～260 ℃; Three district's temperature are 210～260 ℃; Four district's temperature are 210～260 ℃, 210～260 ℃ in five districts, and compound time of delivery in screw rod is 0.5～1 minute.
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| CN103980680A (en) * | 2014-05-31 | 2014-08-13 | 全椒祥瑞塑胶有限公司 | Halogen-free flame retardant plastic |
| CN105647134A (en) * | 2016-03-06 | 2016-06-08 | 贝克兰(厦门)新材料有限公司 | Flame-retardant glass fiber reinforced PBT (polybutylene terephthalate) with high glow wires and high CTI (comparative tracking index) value and method for preparing flame-retardant glass fiber reinforced PBT |
| CN106084686A (en) * | 2016-08-25 | 2016-11-09 | 深圳市高科塑化有限公司 | Charging pile CTI high glow-wire PBT composite and preparation method thereof |
| CN109971138A (en) * | 2019-03-22 | 2019-07-05 | 江门市德山复合材料科技有限公司 | A kind of selfreparing PCBT composite material and preparation method |
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| CN103467932A (en) * | 2013-08-20 | 2013-12-25 | 杨柏容 | PET flame-retardant film master batch, preparation method of PET flame-retardant film master batch and PET flame-retardant film product |
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| CN106084686A (en) * | 2016-08-25 | 2016-11-09 | 深圳市高科塑化有限公司 | Charging pile CTI high glow-wire PBT composite and preparation method thereof |
| CN109971138A (en) * | 2019-03-22 | 2019-07-05 | 江门市德山复合材料科技有限公司 | A kind of selfreparing PCBT composite material and preparation method |
| CN109971138B (en) * | 2019-03-22 | 2021-08-17 | 江门市德山复合材料科技有限公司 | Self-repairing PCBT composite material and preparation method thereof |
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