CN107573653A - A kind of high GWIT flame-retardant PBTs reinforcing material and preparation method thereof, application - Google Patents
A kind of high GWIT flame-retardant PBTs reinforcing material and preparation method thereof, application Download PDFInfo
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- CN107573653A CN107573653A CN201710648286.8A CN201710648286A CN107573653A CN 107573653 A CN107573653 A CN 107573653A CN 201710648286 A CN201710648286 A CN 201710648286A CN 107573653 A CN107573653 A CN 107573653A
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Abstract
The invention discloses a kind of fire-retardant booster stage PBT material for high-voltage great-current working environment and preparation method thereof, application.The preparation method of the alloy material is specially：By 50 55 mass parts PBT resins, 0.1 0.2 mass parts antioxidant, 0.3 0.5 mass parts lubricants are uniformly mixed as mixture A；8~10 mass parts bromide fire retardants, 2 parts of antimony oxides, 58 mass parts compound flame retardants are well mixed to form mixture B；Mixture A is added in extruder from main spout, mixture B is added in extruder with side feeding machine in side spout, 25~30 parts of long glass fibres are fed by way of being involved in naturally in side spout downstream simultaneously, at a temperature of 220~240 DEG C, extruded with 300~450rpm speed, water cooling, drying, pelletizing, obtain the enhancing flame-retardant PBT material for high voltage electrical connector.The alloy material has following excellent performance：Temperature tolerance is good, stability is strong, glowing filament ignition temperature is high, excellent in mechanical performance.
Description
Technical field
The invention belongs to technical field of polymer materials, more particularly to a kind of enhancing suitable for high voltage electrical connector
Flame-retardant PBT material and preparation method thereof, application.
Background technology
PBT plastic refers to a kind of plastics being made up of using polybutylene terephthalate (PBT) main body, and the plastics have excellent
Good mechanical performance, high mechanical strength, fatigue durability and dimensional stability are high, and creep is also small, though under the high temperature conditions these
Premium properties also seldom changes.The enhancing obtained by melt blending means addition glass fibre and flame-retardant additive is fire-retardant
PBT material, there is higher mechanical performance and heat-resistant quality, largely applied to various electronic apparatus connectors, high voltage/super
The fields such as high voltage appliance switch part.
GWIT (glow-wire ignition temperature, the warm-natured degree of glow wire ignition) refers to than " continuously three times
Experiment will not cause maximum temperature high 25K at the top of the glowing filament of the test specimen ignition of specific thickness (900 DEG C~960 DEG C it
Between high 30K) " temperature.
Glow wire ignition it is warm-natured degree be judge in the presence of high-voltage large current, surface of plastic products close to/
Contact may caused by short trouble localized hyperthermia's metallic conductor and a test event artificially proposing.Moulded in test process
Material test sample (will can be manually set) resistance wire with a high fever and contact certain time, observe in contact process and depart from high fever
Combustion case after resistance wire simultaneously records corresponding data.Glowing filament combustion test is different from common UL flame retardant ratings, the former
It is the combustion experiment for simulating high-temperature metal conductor contact plastic products, and naked light is not present；The latter is that simulation naked light has situation
The combustion case of lower plastic products.
The flame-retardant enhanced PBT material species of commercialization at present is many, but can reach compared with high-glowing-filament-temperature flame-retardancy grade
PBT enhancing fire proofings are simultaneously few, and small part grade is by largely adding fire retardant, sacrificing mechanical property to obtain high glow-wire
Flame-retarding characteristic (such as glowing filament anti-flammability temperature reaches 875 degree even grade of the above), it is all defective in practical application.
The content of the invention
The primary and foremost purpose of the present invention is the disadvantages mentioned above and deficiency for overcoming prior art, there is provided it is big that one kind is used for high voltage
The flame-retardant PBT reinforcing material used under current work environment.
Another object of the present invention is to provide a kind of new fire-retardant thinking, the thinking can be that raising fire proofing is scorching hot
Silk performance provides effective instruct.
Another object of the present invention is to carry to develop a kind of flame-retardant PBT reinforcing material of high CTI (voltage breakdown) characteristic
For formula basis.
The above-mentioned purpose of the present invention is to be achieved through the following technical solutions：
A kind of high GWIT flame-retardant PBTs reinforcing material, including composition according to the mass fraction as follows：50~55 parts of PBT resin,
25~30 parts of glass fibre, bromide fire retardant 8-10 parts, assist 2 parts of fire retardant (antimony oxide), compound flame retardant FR60 5-
8 parts, 0.1~0.2 part of high-efficiency anti-oxidant, 0.3~0.5 part of lubricant；
Described PBT resin is 15~30g/10min (250 DEG C, 2.16kg) selected from melt mass flow rate (MFR),
The PBT polyester section of viscosity 1.0；
Described glass fibre is preferably megalith 988A (14 micron diameters, 2000TEX)；
Described bromide fire retardant enters brominated epoxy resin (CXB-400S) selected from South Korea's space, bromine content 48%-50%, divides
Son amount 2000；
Described assistance fire retardant is preferably flash star board antimony oxide (purity>99.5%)；
Described compound flame retardant FR60 is selected from MPP classes halogen-free flame retardants (melamine pyrophosphate, self-control)；
Described high-efficiency anti-oxidant be 1076 (β-positive octadecanol ester of (3,5- di-tert-butyl-hydroxy phenyls) propionic acid) with
626 (double (2,4- DI-tert-butylphenol compounds) pentaerythritol diphosphites) are according to 2:The mixture of 1 mass ratio composition；
Described lubricant is in polysiloxane-based compound, stearic acid ester type compound, stearic amide class compound
One kind or its combination；
Described polysiloxane-based compound is preferably dimethyl silicone polymer, and viscosity is more than 10 × 106mm2/s；
Described stearic acid ester type compound is preferably pentaerythritol stearate (PETS)；
Described stearic amide class compound is preferably ethylene bis stearic acid amide (EBS)；
The preparation method of above-mentioned high GWIT flame-retardant PBTs reinforcing material, comprises the following steps：According to mass fraction meter, by 50-
55 parts of PBT resins, 0.1-0.2 part high-efficiency anti-oxidants, 0.3-0.5 parts lubricant are uniformly mixed as mixture A；By 8~10 parts
Bromide fire retardant, 2 parts of assistance fire retardant antimony oxides, 5-8 part compound flame retardants FR60 is well mixed to form mixture B；Will
Mixture A is added in extruder from main spout, and mixture B is added in extruder with side feeding machine from side spout, while 25
~30 parts of long glass fibres are fed by way of being involved in naturally in side spout downstream, at a temperature of 220~240 DEG C, with 300
~450rpm speed is extruded, and water cooling, drying, pelletizing, obtains the enhancing flame-retardant PBT material for high voltage electrical connector.
Described extruder is double screw extruder, draw ratio 40.
Above-mentioned high GWIT flame-retardant PBTs reinforcing material is used for high-voltage great-current electrical connector (such as connector lug, electric switch)
Application.
The present invention is had the following advantages relative to prior art and beneficial effect：
(1) provided by the present invention for the formula for strengthening flame-retardant PBT material of high voltage electrical connector, collocation is reasonable,
The enhancing fire proofing that ensure that to obtain has excellent performance：Using PBT as material of main part, aid in 25-30 mass parts glass
Fiber, it ensure that material overall heatproof and mechanical property；Compound flame retardant can decomposite largely when overheat condition occurs
Non-flammable inert gas, reduce and even prevent the chance that burning occurs；Flame retardant brominated epoxy resin and antimony oxide energy
Enough ensure that material has retarded combustion when overheat causes ignition or even blocks the ability of combustion phenomena；It is obstructed using larger amount of
Phenolic compound and phosphite ester compound compound as high-efficiency anti-oxidant, be greatly improved material thermo-oxidative stability and
The thermal degradation of material is reduced, adds and heat resistance moderate with PBT compatibilities preferable lubricant PETS, EBS and poly- diformazan in right amount
Radical siloxane, during material machine-shaping, good interior lubrication and outer lubrication are played, surface quality can be obtained more
Good Injection moulded part.
(2) the enhancing flame-retardant PBT material of high voltage electrical connector provided by the invention is under the conditions of 250 DEG C and 2.16kg
Melt mass flow rate (MFR) is 8-10g/10min；PBT strengthens fire proofing at 240-260 DEG C through injection molding process
The product of injection, lustrous surface is good, and dimensional stability is good and the feelings of fracture, warpage or deformation do not occur in plug is tested
Condition.
(3) material mixing can be made evenly using two step mixing methods and side material feeding process when the present invention prepares material, resisted
Oxygen agent is reduced in the loss of extruder, so as to retain more antioxidant, it is played a role in follow-up machine-shaping.
Embodiment
With reference to embodiment, the present invention is described in further detail, but the implementation of the present invention is not limited to this.
The formula of embodiment 1~3 in parts by weight is as follows：
The embodiment 1-3 formula tables of table 1
| Embodiment | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| PBT | 53.3 | 53.3 | 53.3 |
| Glass fibre | 28 | 28 | 28 |
| BEO (brominated epoxy) | 9 | 10 | 11 |
| Antimony oxide | 2 | 2 | 2 |
| FR60 | 7 | 6 | 5 |
| High-efficiency anti-oxidant | 0.2 | 0.2 | 0.2 |
| Lubricant | 0.5 | 0.5 | 0.5 |
According to the formula of embodiment 1,2,3, by the PBT resin of given mass parts, high-efficiency anti-oxidant, lubricant uniformly mixes
As mixture A；Given mass parts bromide fire retardant, antimony oxide, compound flame retardant are well mixed and form mixture B；Will
Mixture A is added in extruder from main spout, and mixture B is added in extruder with side feeding machine in side spout, simultaneously will
Long glass fibres is fed by way of being involved in naturally in side spout downstream, at a temperature of 220~240 DEG C, with 300~
450rpm speed is extruded by double screw extruder (draw ratio 40), and water cooled, dry, pelletizing produces target product.
The formula of comparative example 1-3 in parts by weight is as follows：
The comparative example 1-3 formula tables of table 2
| Comparative example | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| PBT (%) | 52.3 | 52.3 | 81.3 |
| Glass fibre (%) | 28 | 28 | 28 |
| BEO (brominated epoxy) | 15 | 0 | 0 |
| Antimony oxide | 4 | 0 | 0 |
| FR60 | 0 | 19 | 0 |
| High-efficiency anti-oxidant | 0.2 | 0.2 | 0.2 |
| Lubricant | 0.5 | 0.5 | 0.5 |
The reinforcing material that embodiment 1~3 and comparative example 1~3 are prepared is detected.It is first according to same injection
(injection molding machine nozzle, leading portion, stage casing and back segment temperature are respectively 250 DEG C, 245 DEG C, 245 DEG C, 220 DEG C to condition, and screw in injection molding machine turns
Speed is 60rpm, and mold temperature is 60 DEG C, injection pressure 55Mpa, and injection time is 3 seconds, dwell pressure 50Mpa, during pressurize
Between be 8 seconds, cool time is 10 seconds, back pressure 10Mpa) prepare test bars, specific physical property detection project is as follows：
Tensile strength：Tested according to the standards of ISO 527, batten size (mm)：135 × 10 × 4, draw speed is
50mm/min。
Bending strength：Tested according to the standards of ISO 178, batten size (mm)：80 × 10 × 4, rate of bending is
2mm/min。
Izod notched impact strength：Tested according to the standards of ISO 179, batten size (mm)：80×10×4；Lack
Mouth type is A classes, and indentations bottom residue width is 8.0 ± 0.2mm.
Melt flow rate (MFR)：Tested according to ISO1133 standards, 250 DEG C, 2.16kg.
UL94 flame retardant ratings：Grading test is carried out according to UL94.
The warm-natured degree of glow wire ignition：According to IEC 60695-2-13:2000 are tested.
The testing result of sample is as shown in the table：
The performance comparison of the embodiment of table 3 and comparative example
As seen from Table 3, embodiment 1-3 uses increase bromide fire retardant brominated epoxy resin and association on the basis of the present invention
The material property that the ratio of auxiliary flame retardant antimony oxide is obtained is compared, and mechanical property and flame retardant rating have no too big difference,
But glowing filament ignition temperature has the situation of reduction, illustrate that compound flame retardant has for the glowing filament ignition temperature for improving material
Apparent effect；Comparative example 1 eliminates compound flame retardant, though mechanical property is improved, glowing filament ignition temperature is reduced to
750℃；Comparative example 2 eliminates bromide fire retardant, and mechanical property deterioration is serious, and glowing filament ignition temperature is also only up to 800 DEG C；
And comparative example 3 is not added with any fire retardant, glow wire temperature is even reduced to 550 degree, and without flame-retarding characteristic.
In summary, the enhancing flame-retardant PBT material of high voltage electrical connector of the invention have moderate mobility and
Preferable hot-air aging resistance, it can meet required heat-resisting, fire-retardant during High-Voltage Electrical Appliances operation and with prevention line short hair
Ignition phenomenon is overheated caused by heat.
Above-described embodiment is the preferable embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any Spirit Essences without departing from the present invention with made under principle change, modification, replacement, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (7)
1. a kind of high GWIT flame-retardant PBTs reinforcing material, it is characterised in that including following composition according to the mass fraction：PBT resin
50~55 parts, 25~30 parts of glass fibre, bromide fire retardant 8-10 parts, assist 2 parts of fire retardant antimony oxide, compound flame retardant
FR60 5-8 parts, 0.1~0.2 part of high-efficiency anti-oxidant, 0.3~0.5 part of lubricant；
It is 15~30g/10min, viscosity 1.0 under the conditions of 250 DEG C, 2.16kg that the PB resins, which are selected from melt mass flow rate,
PBT polyester section；
The glass fibre is selected from megalith 988A, 14 micron diameters, 2000TEX；
The bromide fire retardant enters brominated epoxy resin, bromine content 48%-50%, molecular weight 2000 selected from South Korea's space；
The assistance fire retardant is selected from flash star board antimony oxide, purity>99.5%；
The compound flame retardant FR60 is selected from MPP class melamine pyrophosphates；
The high-efficiency anti-oxidant is β-positive octadecanol ester of (3,5- di-tert-butyl-hydroxy phenyls) propionic acid and double (uncles of 2,4- bis-
Butylphenol) pentaerythritol diphosphites are according to 2:The mixture of 1 mass ratio composition；
The lubricant is one kind in polysiloxane-based compound, stearic acid ester type compound, stearic amide class compound
Or its combination.
A kind of 2. high GWIT flame-retardant PBTs reinforcing material according to claim 1, it is characterised in that：It is described polysiloxane-based
Compound is selected from dimethyl silicone polymer, and viscosity is more than 10 × 106mm2/s。
A kind of 3. high GWIT flame-retardant PBTs reinforcing material according to claim 1, it is characterised in that：The stearic acid esters
Compound is selected from pentaerythritol stearate.
A kind of 4. high GWIT flame-retardant PBTs reinforcing material according to claim 1, it is characterised in that：The stearic amide
Class compound is selected from ethylene bis stearic acid amide.
5. a kind of preparation method of high GWIT flame-retardant PBTs reinforcing material, it is characterised in that comprise the following steps：According to quality point
Number meter, by 50-55 parts PBT resin, 0.1-0.2 part high-efficiency anti-oxidants, 0.3-0.5 parts lubricant is uniformly mixed as mixture A；
By 8~10 parts of bromide fire retardants, 2 parts of assistance fire retardant antimony oxides, 5-8 part compound flame retardants FR60 is well mixed formed it is mixed
Compound B；Mixture A is added in extruder from main spout, mixture B adds extruder with side feeding machine from side spout
In, while 25~30 parts of long glass fibres are fed by way of being involved in naturally in side spout downstream, in 220~240 DEG C of temperature
Under degree, extruded, water cooling, drying, pelletizing, obtained fire-retardant for the enhancing of high voltage electrical connector with 300~450rpm speed
PBT material.
A kind of 6. preparation method of high GWIT flame-retardant PBTs reinforcing material according to claim 5, it is characterised in that：It is described
Extruder is double screw extruder, draw ratio 40.
7. high GWIT flame-retardant PBTs reinforcing material described in claim 1-4 is used for the application of high-voltage great-current electrical connector.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110016209A (en) * | 2019-04-16 | 2019-07-16 | 武汉顺威赛特工程塑料有限公司 | A kind of GWIT850 DEG C of enhancing flame-retardant PBT and its preparation method and application |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101928449A (en) * | 2010-09-06 | 2010-12-29 | 上海俊尔新材料有限公司 | High glowing filament ignition temperature inflaming retarding reinforced poly(butylene terephthalate) |
| 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 |
-
2017
- 2017-08-01 CN CN201710648286.8A patent/CN107573653A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101928449A (en) * | 2010-09-06 | 2010-12-29 | 上海俊尔新材料有限公司 | High glowing filament ignition temperature inflaming retarding reinforced poly(butylene terephthalate) |
| 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 |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110016209A (en) * | 2019-04-16 | 2019-07-16 | 武汉顺威赛特工程塑料有限公司 | A kind of GWIT850 DEG C of enhancing flame-retardant PBT and its preparation method and application |
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