CN102532818A - Carbon fiber-glass fiber composite enhanced flame-retardant PBT (Polybutylece Terephthalate) material and preparation method thereof - Google Patents

Carbon fiber-glass fiber composite enhanced flame-retardant PBT (Polybutylece Terephthalate) material and preparation method thereof Download PDF

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Publication number
CN102532818A
CN102532818A CN2010105913982A CN201010591398A CN102532818A CN 102532818 A CN102532818 A CN 102532818A CN 2010105913982 A CN2010105913982 A CN 2010105913982A CN 201010591398 A CN201010591398 A CN 201010591398A CN 102532818 A CN102532818 A CN 102532818A
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parts
pbt
retardant pbt
glass fiber
retardant
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CN102532818B (en
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查敏
陈永东
张祥福
周文
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Shanghai Pret Composites Co Ltd
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Shanghai Pret Composites Co Ltd
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    • B29C47/92

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Abstract

The invention discloses a carbon fiber-glass fiber composite enhanced flame-retardant PBT (Polybutylece Terephthalate) material and a preparation method thereof, which can be applied in the fields of automobiles, electronics/electrical appliances and the like and belong to the technical field of high-polymer materials. The carbon fiber-glass fiber composite enhanced flame-retardant PBT material comprises the following components in parts by weight: 50-75 parts of PBT resin, 10-25 pats of chopped glass fiber, 5-20 parts of carbon fiber, 2-7 parts of a toughening compatilizer, 10-15 parts of bromide, 2-5 parts of antimonous oxide, 0.1-0.5 part of a nucleating agent and 0.2-5 parts of other additives. In the invention, carbon fiber is introduced on the basis of glass fiber enhancement, and the flame-retardant PBT material is subjected to composite enhancing modification. The composite material prepared with the method has higher mechanical property than apure glass fiber enhanced flame-retardant PBT material; and a finished piece processed and molded by using the composite material is attractive, has superior conductivity, superior size stability, high practicability and high commercial value, and can be applied to a cover plate of an injection-molded money counter.

Description

The compound enhancing flame-retardant PBT of the fine glass of carbon material and preparation method thereof
Technical field
The present invention relates to the compound enhancing flame-retardant PBT of the fine glass of a kind of carbon material and preparation method thereof, can be applicable to fields such as automobile and electronics/electrical equipment, belong to technical field of polymer materials.
Background technology
Polyester is owing to forming process property, electrical insulating property, excellent properties such as heat-resisting are widely used in electronics, electrical equipment, household electric appliances.Because these industries have strict regulation to combustion safety, so flame retardant polyester becomes an important kind of polyester modification.Flame-retardant reinforced polyester is a main products in flame retardant polyester, and the performance of existing glass-fiber-reinforced polyester has good resistance to flame again.Correlative study for flame-retardant enhanced PBT material is many with report.
Patent CN101817972A for example, the name of this application for a patent for invention is called " a kind of flame-retardant enhanced PBT material and preparation method thereof ".This material is made up of following component by weight percentage: PBT resin 45~60%; Bromide fire retardant 3~10%; Phosphor nitrogen combustion inhibitor 1~10%; Inorganic combustion inhibitor 1~5%.Toughner 2~5%; Spun glass 20~35%; Lubricant 0.3~1%; Oxidation inhibitor 0.1~0.6%.Not only glowing filament ignition temperature is high for this invention flame-retardant enhanced PBT material, and phase ratio creepage tracking index is high, has better mechanical property simultaneously, can be widely used in unattended field of electronics.
Patent CN101225220A and for example, patent name is " fire-retardant enhancing polybutylene terephthalate mixture and a working method ".This mixture is formulated by PBT, other polyester, spun glass, bromide, Antimony Trioxide: 99.5Min, toughness reinforcing, compatilizer, oxidation inhibitor, anti-dripping agent, nucleator.This invention preparation technology is simple, cost is low.
Summary of the invention
The object of the invention aims to provide a kind of high-performance, the compound enhancing flame-retardant PBT of the fine glass of anlistatig carbon material and preparation method thereof.
The object of the invention can be realized through following technical scheme.
The compound enhancing flame-retardant PBT of the fine glass of carbon material, by weight, its component and content are:
50~75 parts of PBT resins
10~25 parts of short glass fibers
5~20 parts on thomel
2~7 parts of toughness reinforcing compatilizers
10~15 parts of bromides
2~5 parts of Antimony Trioxide: 99.5Mins
0.1~0.5 part of nucleator
0.2~5 part of other additive.
Described PBT resin is a polybutylene terephthalate, and its specific density is 1.31~1.35, and fusing point is 220~230 ℃, and viscosity is 0.6~0.9P.S.
Described short glass fiber is that length is the short glass fiber of 3-4.5mm.
Described thomel is to be the short carbon fibre of 6mm by the length that polyacrylonitrile fibre is transformed through bakingout process.
Described toughness reinforcing compatilizer is ethylene-methyl methacrylate butyl ester and glycidyl acrylate multipolymer.
Described bromide is a brominated aromatic polymer class fire retardant.
Described Antimony Trioxide: 99.5Min is melt temperature 640-670 ℃, and outward appearance is the powder of white.
Described nucleator is aromatic base phosphates or talcum powder.
Described other additives comprise oxidation inhibitor, fast light according to auxiliary agent, shades of colour additive, various ester class or fatty acid lubricant etc.
The compound enhancing flame-retardant PBT of the fine glass of this carbon preparation methods, its concrete steps are:
(1) takes by weighing raw material by weight ratio;
(2) the evenly mixed back of PBT resin, toughness reinforcing compatilizer, bromide, Antimony Trioxide: 99.5Min, nucleator, oxidation inhibitor and lubricant is got into twin screw extruder, add from the side direction spout behind short glass fiber and the thomel uniform mixing.Complete processing is following: 160~190 ℃ of district's temperature, 225~235 ℃ of two district's temperature, 225~235 ℃ of three district's temperature, 225~235 ℃ of four district's temperature, 220~230 ℃ of five district's temperature, 440~470 rev/mins of engine speeds, 10-60 rev/min of side feeding rotating speed;
(3) extrude the preparation method that postcooling, drying, pelletizing promptly get the compound enhancing flame-retardant PBT of the fine glass of carbon.
The present invention introduces thomel on the former glass enhanced basis, to the compound enhancing modified of flame-retardant PBT material.Matrix material by this law preparation has higher mechanical property than pure fiberglass reinforced fire retardant PBT material; And by the product of its machine-shaping appearance looks elegant not only; And have good electroconductibility and dimensional stability, have very big practicality and commercial value, can be used for injection moulding counting cover plate.
Embodiment
Below in conjunction with embodiment, the present invention is done further explain.
In Example formulations, the PBT resin trade mark is 4500, and Jiangsu San Fangxiang produces.
Described short glass fiber is Chongqing glass ECS 303A.
Described thomel is the Japanese eastern HT C493 of nation, and length is 6mm.
Described toughness reinforcing compatilizer is Elvaloy PTW, du pont company production.
Described bromide is a TDE, and product grade is 8010, refined precious production of the U.S..
Described Antimony Trioxide: 99.5Min is that Hunan Lengshuijiang City Xikuangshan Shanxing Antimony Industry Co., Ltd produces.
Described nucleator is NA21, and chemical name is methylene-bis (2, a 4-di-tert-butyl-phenyl) phosphagel phosphaljel, is produced by Adeka Palmerole company.
Described other additives are oxidation inhibitor 2450 and 168 (1: 1).Wherein oxidation inhibitor 2450 is produced for Korea S Songyuan City, and trade names are Songnox 2450, and chemical name is triethylene glycol ether-two (3-tertiary butyl-4-hydroxy-5-aminomethyl phenyl) propionic ester.Oxidation inhibitor 168 is produced for Ciba company, and trade names are Irgafos 168, and chemical name is three (2, the 4-di-tert-butyl-phenyl) phosphorous acid ester.
Described lubricant is that the good Zhuo Huagong ltd in Shanghai produces for OP wax.
PBT resin, toughness reinforcing compatilizer, bromide, Antimony Trioxide: 99.5Min, nucleator, oxidation inhibitor and lubricant are got into twin screw extruder after dried mixed 3~5 minutes in super mixer; Add from the side direction spout behind short glass fiber and the thomel uniform mixing; Complete processing is: 160~190 ℃ of district's temperature, 225~235 ℃ of two district's temperature, 225~235 ℃ of three district's temperature; 225~235 ℃ of four district's temperature; 220~230 ℃ of five district's temperature, 440~470 rev/mins of engine speeds, 10-60 rev/min of side feeding rotating speed.The product performance testing method:
Tensile property is pressed the ISO527 method, and draw speed is 50mm/min, and batten is of a size of 150*10*4mm.
Bending property is pressed the ISO178 method, and trial speed is 2mm/min, and batten is of a size of 80*10*4mm, span 64mm.
Breach Charpy shock strength is pressed the ISO179 method, and batten is of a size of 80*10*4mm, and notch depth is 1/5th of a sample thickness.
Surface resistivity adopts the surface resistivity appearance to measure, and batten is of a size of 150*100*3.
Introduce embodiments of the invention below:
Embodiment 1
With 57 parts of PBT resins; 5 parts of toughness reinforcing compatilizer PTW, 10 parts of TDEs, 3 parts of Antimony Trioxide: 99.5Mins, 0.3 part of nucleator NA21,2,450 0.1 parts in oxidation inhibitor, 168 0.2 parts in oxidation inhibitor, 0.5 part of mixing of lubricant OP wax are placed in the twin screw extruder and melt extrude through 225~235 ℃; And with adding from the side direction spout after 15 parts of short glass fiber ECS 303A and 10 parts of mixing of thomel HTC493, matrix material is processed in granulation.
Embodiment 2
With 57 parts of PBT resins; 5 parts of toughness reinforcing compatilizer PTW, 10 parts of TDEs, 3 parts of Antimony Trioxide: 99.5Mins, 0.3 part of nucleator NA21,2,450 0.1 parts in oxidation inhibitor, 168 0.2 parts in oxidation inhibitor, 0.5 part of mixing of lubricant OP wax are placed in the twin screw extruder and melt extrude through 225~235 ℃; And with adding from the side direction spout after 20 parts of short glass fiber ECS 303A and 5 parts of mixing of thomel HTC493, matrix material is processed in granulation.
Embodiment 3
With 57 parts of PBT resins; 5 parts of toughness reinforcing compatilizer PTW, 10 parts of TDEs, 3 parts of Antimony Trioxide: 99.5Mins, 0.3 part of nucleator NA21,2,450 0.1 parts in oxidation inhibitor, 168 0.2 parts in oxidation inhibitor, 0.5 part of mixing of lubricant OP wax are placed in the twin screw extruder and melt extrude through 225~235 ℃; And with adding from the side direction spout after 10 parts of short glass fiber ECS 303A and 15 parts of mixing of thomel HTC493, matrix material is processed in granulation.
Embodiment 4
With 62 parts of PBT resins; 5 parts of toughness reinforcing compatilizer PTW, 10 parts of TDEs, 3 parts of Antimony Trioxide: 99.5Mins, 0.3 part of nucleator NA21,2,450 0.1 parts in oxidation inhibitor, 168 0.2 parts in oxidation inhibitor, 0.5 part of mixing of lubricant OP wax are placed in the twin screw extruder and melt extrude through 225~235 ℃; And with adding from the side direction spout after 10 parts of short glass fiber ECS 303A and 10 parts of mixing of thomel HTC493, matrix material is processed in granulation.
Embodiment 5
With 62 parts of PBT resins; 5 parts of toughness reinforcing compatilizer PTW, 10 parts of TDEs, 3 parts of Antimony Trioxide: 99.5Mins, 0.3 part of nucleator NA21,2,450 0.1 parts in oxidation inhibitor, 168 0.2 parts in oxidation inhibitor, 0.5 part of mixing of lubricant OP wax are placed in the twin screw extruder and melt extrude through 225~235 ℃; And with adding from the side direction spout after 15 parts of short glass fiber ECS 303A and 15 parts of mixing of thomel HTC493, matrix material is processed in granulation.
Comparative Examples 1
With 57 parts of PBT resins; 5 parts of toughness reinforcing compatilizer PTW, 10 parts of TDEs, 3 parts of Antimony Trioxide: 99.5Mins, 0.3 part of nucleator NA21,2,450 0.1 parts in oxidation inhibitor, 168 0.2 parts in oxidation inhibitor, 0.5 part of mixing of lubricant OP wax are placed in the twin screw extruder and melt extrude through 225~235 ℃; And from 25 parts of side direction spout adding short glass fiber ECS 303A, matrix material is processed in granulation.
Comparative Examples 2
With 62 parts of PBT resins; 5 parts of toughness reinforcing compatilizer PTW, 10 parts of TDEs, 3 parts of Antimony Trioxide: 99.5Mins, 0.3 part of nucleator NA21,2,450 0.1 parts in oxidation inhibitor, 168 0.2 parts in oxidation inhibitor, 0.5 part of mixing of lubricant OP wax are placed in the twin screw extruder and melt extrude through 225~235 ℃; And from 20 parts of side direction spout adding short glass fiber ECS 303A, matrix material is processed in granulation.
Comparative Examples 3
With 52 parts of PBT resins; 5 parts of toughness reinforcing compatilizer PTW, 10 parts of TDEs, 3 parts of Antimony Trioxide: 99.5Mins, 0.3 part of nucleator NA21,2,450 0.1 parts in oxidation inhibitor, 168 0.2 parts in oxidation inhibitor, 0.5 part of mixing of lubricant OP wax are placed in the twin screw extruder and melt extrude through 225~235 ℃; And from 30 parts of side direction spout adding short glass fiber ECS 303A, matrix material is processed in granulation.
The mechanical property of table 1 flame-retardant reinforced PBT
Test result by embodiment 1~embodiment 5 and Comparative Examples 1~Comparative Examples 3 can be found out; Carbon fibre and the compound enhancing flame-retardant PBT of glass material strengthen the flame-retardant PBT material than pure glass dimension and have higher tensile strength and modulus; And along with the raising of the fine ratio of carbon, the strength of materials and modulus improve significantly.Compound in addition enhancing flame-retardant PBT material has excellent conductivity.When the fine content of carbon was 10%, the surface resistivity of material just can reduce to 10 3Ω becomes electro-conductive material, is applicable to the preparation of antistatic material.

Claims (10)

1. the compound enhancing flame-retardant PBT of the fine glass of carbon material, it is characterized in that: by weight, its component and content are:
50~75 parts of PBT resins
10~25 parts of short glass fibers
5~20 parts on thomel
2~7 parts of toughness reinforcing compatilizers
10~15 parts of bromides
2~5 parts of Antimony Trioxide: 99.5Mins
0.1~0.5 part of nucleator
0.2~5 part of other additive.
2. the compound enhancing flame-retardant PBT of the fine glass of carbon according to claim 1 material, it is characterized in that: described PBT resin is a polybutylene terephthalate, and its specific density is 1.31~1.35, and fusing point is 220~230 ℃, and viscosity is 0.6~0.9P.S.
3. the compound enhancing flame-retardant PBT of the fine glass of carbon according to claim 1 material, it is characterized in that: described short glass fiber is that length is the short glass fiber of 3-4.5mm.
4. described thomel is to be the short carbon fibre of 6mm by the length that polyacrylonitrile fibre is transformed through bakingout process.
5. the compound enhancing flame-retardant PBT of the fine glass of carbon according to claim 1 material, it is characterized in that: described toughness reinforcing compatilizer is ethylene-methyl methacrylate butyl ester and glycidyl acrylate multipolymer.
6. the compound enhancing flame-retardant PBT of the fine glass of carbon according to claim 1 material, it is characterized in that: described bromide is a brominated aromatic polymer class fire retardant.
7. the compound enhancing flame-retardant PBT of the fine glass of carbon according to claim 1 material, it is characterized in that: described Antimony Trioxide: 99.5Min is melt temperature 640-670 ℃, outward appearance is the powder of white.
8. the compound enhancing flame-retardant PBT of the fine glass of carbon according to claim 1 material, it is characterized in that: described nucleator is aromatic base phosphates or talcum powder.
9. the compound enhancing flame-retardant PBT of the fine glass of carbon according to claim 1 material is characterized in that: described other additives comprise oxidation inhibitor, fast light according to auxiliary agent, shades of colour additive, various ester class or fatty acid lubricant.
10. prepare the method for the compound enhancing flame-retardant PBT of the fine glass of the said carbon of claim 1 material, it is characterized in that: its concrete steps are:
(1) takes by weighing raw material by weight ratio;
(2) the evenly mixed back of PBT resin, toughness reinforcing compatilizer, bromide, Antimony Trioxide: 99.5Min, nucleator, oxidation inhibitor and lubricant is got into twin screw extruder, add from the side direction spout behind short glass fiber and the thomel uniform mixing.Complete processing is following: 160~190 ℃ of district's temperature, 225~235 ℃ of two district's temperature, 225~235 ℃ of three district's temperature, 225~235 ℃ of four district's temperature, 220~230 ℃ of five district's temperature, 440~470 rev/mins of engine speeds, 10-60 rev/min of side feeding rotating speed;
(3) extrude the preparation method that postcooling, drying, pelletizing promptly get the compound enhancing flame-retardant PBT of the fine glass of carbon.
CN201010591398.2A 2010-12-16 2010-12-16 Carbon fiber-glass fiber composite enhanced flame-retardant PBT (Polybutylece Terephthalate) material and preparation method thereof Active CN102532818B (en)

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103540015A (en) * 2013-09-23 2014-01-29 句容市睿远科技有限公司 Light high-strength flame retardant composite material for high-speed train compartment and preparation method thereof
CN103756266A (en) * 2013-12-20 2014-04-30 南通开普乐工程塑料有限公司 Flame retardant glass fiber reinforced PBT (Polybutylene Terephthalate) composite material and preparation method thereof
CN104151784A (en) * 2013-05-14 2014-11-19 常熟市沈氏塑业有限公司 Nano carbon fiber reinforced polybutylene terephthalate alloy composite material
CN105504702A (en) * 2015-12-24 2016-04-20 广东思汗新材料有限公司 Flame-retardant electric conducting PBT composite material
WO2019033277A1 (en) * 2017-08-15 2019-02-21 南通大学 Magnetic base test tube, syringe rack and storage tray for clean bench use
CN110157163A (en) * 2019-05-27 2019-08-23 福建师范大学 A kind of assorted fibre enhancing r-PET engineering plastics and preparation method thereof
US10633535B2 (en) 2017-02-06 2020-04-28 Ticona Llc Polyester polymer compositions
US11384238B2 (en) 2018-02-08 2022-07-12 Celanese Sales Germany Gmbh Polymer composite containing recycled carbon fibers
CN114736495A (en) * 2022-06-13 2022-07-12 南通开普乐工程塑料有限公司 Carbon fiber reinforced PBT material and preparation method thereof

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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104151784A (en) * 2013-05-14 2014-11-19 常熟市沈氏塑业有限公司 Nano carbon fiber reinforced polybutylene terephthalate alloy composite material
CN103540015A (en) * 2013-09-23 2014-01-29 句容市睿远科技有限公司 Light high-strength flame retardant composite material for high-speed train compartment and preparation method thereof
CN103540015B (en) * 2013-09-23 2015-09-02 句容市睿远科技有限公司 For the Light high-strength flame retardant composite material and preparation method thereof of speed train cars
CN103756266A (en) * 2013-12-20 2014-04-30 南通开普乐工程塑料有限公司 Flame retardant glass fiber reinforced PBT (Polybutylene Terephthalate) composite material and preparation method thereof
CN105504702A (en) * 2015-12-24 2016-04-20 广东思汗新材料有限公司 Flame-retardant electric conducting PBT composite material
US10633535B2 (en) 2017-02-06 2020-04-28 Ticona Llc Polyester polymer compositions
WO2019033277A1 (en) * 2017-08-15 2019-02-21 南通大学 Magnetic base test tube, syringe rack and storage tray for clean bench use
US11384238B2 (en) 2018-02-08 2022-07-12 Celanese Sales Germany Gmbh Polymer composite containing recycled carbon fibers
US11993707B2 (en) 2018-02-08 2024-05-28 Celanese Sales Germany Gmbh Polymer composite containing recycled carbon fibers
CN110157163A (en) * 2019-05-27 2019-08-23 福建师范大学 A kind of assorted fibre enhancing r-PET engineering plastics and preparation method thereof
CN114736495A (en) * 2022-06-13 2022-07-12 南通开普乐工程塑料有限公司 Carbon fiber reinforced PBT material and preparation method thereof

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