CN109867924A - A kind of fire-retardant enhancing PA6/PBT material of high CTI high-impact and preparation method thereof - Google Patents
A kind of fire-retardant enhancing PA6/PBT material of high CTI high-impact and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of high fire-retardant enhancing PA6/PBT materials of CTI high-impact and preparation method thereof, more particularly to technical field of polymer materials, it is described to prepare raw material according to the mass fraction, including following component: 10-45 parts of PA6,10-45 parts of PBT, 10-30 parts of glass fibre, 10-20 parts of composite flame-proof master batch, 1-5 parts of compatible toughening agents, 0.2-1.5 parts of antioxidant, 0.2-2.0 parts of lubricant；The PA6 is polycaprolactam；The PBT is polybutylene terephthalate (PBT)；The composite flame-proof master batch is the mixture of iron red phosphorus master batch 40, melamine polyphosphate 30 and high CTI auxiliary agent 20；The compatible toughening agents are maleic anhydride grafted ethene octene copolymer.The present invention by using PA6 with PBT is compound is prepared into alloy, both effectively combine feature performance benefit, can be realized its mutual supplement with each other's advantages, dimensional stability is improved, meanwhile, composite flame-proof master batch is added, material comprehensive mechanical property is improved, erosion-resisting characteristics and CTI value are increased substantially.
Description
Technical field
The present invention relates to technical field of polymer materials, it is more particularly related to which a kind of high CTI high-impact is fire-retardant
Enhance PA6/PBT material and preparation method thereof.
Background technique
With the rapid development of electronic apparatus industry, industrial electrical equipment, household electrical appliance and car electrics etc. are to high electrical insulating properties
The demand of energy fire-resistant engineering plastics is growing.Such as high-voltage appliance switch, transformer coil frame, high-temperature resistant relay, low pressure
Vacuum contactor, breaker etc., require that flame retardant property is high, electrical insulation capability is good, i.e., phase ratio creepage tracking index (CTI) is high
Thermoplastic engineering plastic.
The patent of invention of 102942739 A of patent application publication CN discloses a kind of high CTI value, the environmental protection of high GWIT value
Flame-proof glass fibre enhances PP material and preparation method thereof, is compared, is being hindered with traditional flame-retardant system using novel flame-retardant compound system
It fires in the identical situation of agent percentage composition, novel built system can make the GWIT value of material improve 50-100 DEG C, can pass through 850
DEG C glowing filament, the addition of glass fibre improve the GWIT value of material significantly, and compatible toughening agents, which are added, improves rushing for material
Performance is hit, antioxygenic property and use of the composition in process can be improved using Hinered phenols antioxidant in antioxidant
Material processing fluidity can be improved using iron oxide as the auxiliary agent for mentioning high CTI value in anti-aging property in the process, and reduction rubs
Coefficient is wiped, slipping is improved, while using dispersibility is preferable, the residence time is short, shearing is slightly weak under specific processing conditions
Combination, can prevent fire retardant from decomposing, to ensure that the quality of material is stablized.
But it is in actual use, still there is more disadvantage, as halogen-free flameproof enhancing alloy has comprehensive mechanical property
Can be poor the disadvantages of.
Summary of the invention
In order to overcome the drawbacks described above of the prior art, the present invention provides a kind of fire-retardant enhancing PA6/PBT material of high CTI high-impact
Material and preparation method thereof, by using PA6 with PBT is compound is prepared into alloy, both effectively combine feature performance benefit, can be realized it
Have complementary advantages, improves dimensional stability, meanwhile, composite flame-proof master batch is added, improves material comprehensive mechanical property, increases substantially
Erosion-resisting characteristics, CTI value, to solve the problems mentioned in the above background technology.
To achieve the above object, the invention provides the following technical scheme: a kind of fire-retardant enhancing PA6/PBT of high CTI high-impact
Material, it is described to prepare raw material according to the mass fraction, including following component: 10-45 parts of PA6,10-45 parts of PBT, glass fibre
10-30 parts, 10-20 parts of composite flame-proof master batch, 1-5 parts of compatible toughening agents, 0.2-1.5 parts of antioxidant, 0.2-2.0 parts of lubricant；
The PA6 is polycaprolactam；
The PBT is polybutylene terephthalate (PBT)；
The composite flame-proof master batch is the mixing of iron red phosphorus master batch 40, melamine polyphosphate 30 and high CTI auxiliary agent 20
Object；
The compatible toughening agents are maleic anhydride grafted ethene octene copolymer；
The glass fibre includes long glass fibres and short glass fiber, the long glass fibres and short glass fiber
Diameter is 8-15 μm；
The antioxidant includes four (3,5- di-t-butyl -4- hydroxyl) benzenpropanoic acid pentaerythritol esters, three (2, the tertiary fourth of 4- bis-
Base) phenyl-phosphite, N, N '-bis--(3- (3,5- di-tert-butyl-hydroxy phenyl) propiono) hexamethylene diamine；
The lubricant is polyethylene wax, EBS, silicone, silicone oil and combinations thereof.
In a preferred embodiment, the grafting rate of the maleic anhydride grafted ethene octene copolymer is 1.5%.
In a preferred embodiment, the modified glass-fiber that the glass fibre is selected.
In a preferred embodiment, each component mass parts for preparing raw material be respectively 20-40 parts of PA6,
10-30 parts of PBT, 15-30 parts of glass fibre, 10-20 parts of composite flame-proof master batch, 1-5 parts of compatible toughening agents, antioxidant 0.2-1.5
Part, 0.2-2.0 parts of lubricant.
The present invention also provides a kind of preparation method of the fire-retardant enhancing PA6/PBT material of high CTI high-impact, specifically include as
Lower operating procedure:
S1: raw material premix are closed: by the proportion by weight of above-mentioned raw materials, PA6, PBT and compatible toughening agents after taking drying, and
It is placed in high-speed mixer together with antioxidant and lubricant, is sufficiently mixed at normal temperature uniformly, obtains mixture, it is standby
With；
S2: the modification of glass fibre:
(1) glass fibre is placed in working gas is nitrogen, and operating pressure 10-20Pa, discharge power is 80-110W's
100-120s is handled in low-temperature plasma device, obtains pretreated glass fiber；
(2) methacrylic acid and water are mixed by solid-to-liquid ratio (2-6) g:100mL, with 200-400r/min at 80-90 DEG C
Revolving speed stir 20-40min, obtain methacrylic acid solution；
(3) pretreated glass fiber and methacrylic acid solution are mixed by solid-to-liquid ratio (8-12) g:100mL, in 80-90
40-60min is stirred with the revolving speed of 200-400r/min at DEG C, obtained solid is in 80-90 DEG C of vacuum drying 12-18h, to obtain
To modified glass-fiber；
S3: mixture obtained in S1 is added in the double screw extruder from the main spout of double screw extruder,
Meanwhile by the proportion by weight of above-mentioned raw materials, by the modified glass-fiber prepared in S2 and composite flame-proof master batch successively from double
The side spout of screw extruder is added in the double screw extruder, and is uniformly mixed in double screw extruder, is then squeezed
Pelletizing obtains the fire-retardant enhancing PA6/PBT material of high CTI high-impact out.
In a preferred embodiment, the condition mixed in the S1 is 800r/min, mixing time 5-
10min。
In a preferred embodiment, double screw extruder diameter is less than 120mm, double screw extruder in the S3
Host revolution 300-500r/min, barrel temperature are 240-270 DEG C, 20-50 DEG C of sink temperature, and pelletizing is selected in pelletizing in the S2
Machine revolving speed is 400-700r/min.
Technical effect and advantage of the invention:
The resistant to chemical etching of raw material polycaprolactam, the wear-resistant and self-lubrication of the present invention of preparing is all fine, but inhales
Water rate is high, molding shrinkage is big, and the water absorption rate of PBT is low, good stability of the dimension, but easily decomposes under the condition of high temperature and high humidity, resists
Punching performance is poor, by using PA6 with PBT is compound is prepared into alloy, both effectively combine feature performance benefit, can be realized its advantage
Complementation improves dimensional stability, meanwhile, composite flame-proof master batch is added, improves material comprehensive mechanical property, increases substantially anti-impact
Performance and CTI value.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical solution of the present invention is clearly and completely described, it is clear that
Described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on the implementation in the present invention
Example, every other embodiment obtained by those of ordinary skill in the art without making creative efforts belong to
The scope of protection of the invention.
Embodiment 1
A kind of fire-retardant enhancing PA6/PBT material of high CTI high-impact is present embodiments provided, the raw material for preparing is by mass parts
Number meter, including following component: 20 parts of PA6,45 parts of PBT, 15 parts of glass fibre, 10 parts of composite flame-proof master batch, compatible toughening agents 1
Part, 0.2 part of antioxidant, 0.2 part of lubricant.
The present embodiment additionally provides a kind of preparation method of fire-retardant enhancing PA6/PBT material of high CTI high-impact, specifically includes
Following operating procedure:
S1: raw material premix are closed: 20 parts of PA6,45 parts of PBT and 1 part of phases by the proportion by weight of above-mentioned raw materials, after taking drying
Hold toughener, and it is placed in high-speed mixer together with 0.2 part of antioxidant and 0.2 part of lubricant, at normal temperature sufficiently
It is uniformly mixed, obtains mixture, it is spare；
S2: the modification of glass fibre:
(1) glass fibre is placed in working gas is nitrogen, and operating pressure 10-20Pa, discharge power is 80-110W's
100-120s is handled in low-temperature plasma device, obtains pretreated glass fiber；
(2) methacrylic acid and water are mixed by solid-to-liquid ratio (2-6) g:100mL, with 200-400r/min at 80-90 DEG C
Revolving speed stir 20-40min, obtain methacrylic acid solution；
(3) pretreated glass fiber and methacrylic acid solution are mixed by solid-to-liquid ratio (8-12) g:100mL, in 80-90
40-60min is stirred with the revolving speed of 200-400r/min at DEG C, obtained solid is dried in vacuo 12-18h at 80-90 DEG C, thus
Obtain modified glass-fiber；
S3: mixture obtained in S1 is added in the double screw extruder from the main spout of double screw extruder,
Meanwhile by the modified glass-fiber prepared in 15 parts of S2 and 10 parts of composite flame-proof master batches successively from the side feed of double screw extruder
Material mouth is added in the double screw extruder, and is uniformly mixed in double screw extruder, is then squeezed out pelletizing and is obtained high CTI high
The fire-retardant enhancing PA6/PBT material of anti-impact, wherein the condition mixed in S1 is 800r/min, and mixing time is less than 5-10min, and
Double screw extruder diameter is less than 120mm, twin-screw extrusion machine host revolution 300-500r/min, barrel temperature 240 in S3
DEG C, 20-50 DEG C of sink temperature, it is 400-700r/min that pelleter revolving speed is selected in pelletizing in the S2.
Embodiment 2
A kind of fire-retardant enhancing PA6/PBT material of high CTI high-impact is present embodiments provided, the raw material for preparing is by mass parts
Number meter, including following component: 30 parts of PA6,20 parts of PBT, 30 parts of glass fibre, 15 parts of composite flame-proof master batch, compatible toughening agents 3
Part, 0.8 part of antioxidant, 1.2 parts of lubricant.
The present embodiment additionally provides a kind of preparation method of fire-retardant enhancing PA6/PBT material of high CTI high-impact, specifically includes
Following operating procedure:
S1: raw material premix are closed: 30 parts of PA6,20 parts of PBT and 3 part of phases by the proportion by weight of above-mentioned raw materials, after taking drying
Hold toughener, and it is placed in high-speed mixer together with 0.8 part of antioxidant and 1.2 parts of lubricants, at normal temperature sufficiently
It is uniformly mixed, obtains mixture, it is spare；
S2: the modification of glass fibre:
(1) glass fibre is placed in working gas is nitrogen, and operating pressure 10-20Pa, discharge power is 80-110W's
100-120s is handled in low-temperature plasma device, obtains pretreated glass fiber；
(2) methacrylic acid and water are mixed by solid-to-liquid ratio (2-6) g:100mL, with 200-400r/min at 80-90 DEG C
Revolving speed stir 20-40min, obtain methacrylic acid solution；
(3) pretreated glass fiber and methacrylic acid solution are mixed by solid-to-liquid ratio (8-12) g:100mL, in 80-90
40-60min is stirred with the revolving speed of 200-400r/min at DEG C, obtained solid is dried in vacuo 12-18h at 80-90 DEG C, thus
Obtain modified glass-fiber；
S3: mixture obtained in S1 is added in the double screw extruder from the main spout of double screw extruder,
Meanwhile by the modified glass-fiber prepared in 30 parts of S2 and 15 parts of composite flame-proof master batches successively from the side feed of double screw extruder
Material mouth is added in the double screw extruder, and is uniformly mixed in double screw extruder, is then squeezed out pelletizing and is obtained high CTI high
The fire-retardant enhancing PA6/PBT material of anti-impact, wherein the condition mixed in S1 is 800r/min, mixing time 5-10min, and S3
Middle double screw extruder diameter is less than 120mm, twin-screw extrusion machine host revolution 300-500r/min, and barrel temperature is 255 DEG C,
20-50 DEG C of sink temperature, it is 400-700r/min that pelleter revolving speed is selected in pelletizing in the S2.
Embodiment 3
A kind of fire-retardant enhancing PA6/PBT material of high CTI high-impact is present embodiments provided, the raw material for preparing is by mass parts
Number meter, including following component: 40 parts of PA6,10 parts of PBT, 30 parts of glass fibre, 20 parts of composite flame-proof master batch, compatible toughening agents 5
Part, 1.5 parts of antioxidant, 2.0 parts of lubricant.
The present embodiment additionally provides a kind of preparation method of fire-retardant enhancing PA6/PBT material of high CTI high-impact, specifically includes
Following operating procedure:
S1: raw material premix are closed: 40 parts of PA6,10 parts of PBT and 5 part of phases by the proportion by weight of above-mentioned raw materials, after taking drying
Hold toughener, and it is placed in high-speed mixer together with 1.5 parts of antioxidant and 2.0 parts of lubricants, at normal temperature sufficiently
It is uniformly mixed, obtains mixture, it is spare；
S2: the modification of glass fibre:
(1) glass fibre is placed in working gas is nitrogen, and operating pressure 10-20Pa, discharge power is 80-110W's
100-120s is handled in low-temperature plasma device, obtains pretreated glass fiber；
(2) methacrylic acid and water are mixed by solid-to-liquid ratio (2-6) g:100mL, with 200-400r/min at 80-90 DEG C
Revolving speed stir 20-40min, obtain methacrylic acid solution；
(3) pretreated glass fiber and methacrylic acid solution are mixed by solid-to-liquid ratio (8-12) g:100mL, in 80-90
40-60min is stirred with the revolving speed of 200-400r/min at DEG C, obtained solid is dried in vacuo 12-18h at 80-90 DEG C, thus
Obtain modified glass-fiber；
S3: mixture obtained in S1 is added in the double screw extruder from the main spout of double screw extruder,
Meanwhile by the modified glass-fiber prepared in 30 parts of S2 and 20 parts of composite flame-proof master batches successively from the side feed of double screw extruder
Material mouth is added in the double screw extruder, and is uniformly mixed in double screw extruder, is then squeezed out pelletizing and is obtained high CTI high
The fire-retardant enhancing PA6/PBT material of anti-impact, wherein the condition mixed in S1 is 800r/min, and mixing time is greater than 10min, and S3
Middle double screw extruder diameter is less than 120mm, twin-screw extrusion machine host revolution 300-500r/min, and barrel temperature is 270 DEG C,
20-50 DEG C of sink temperature, it is 400-700r/min that pelleter revolving speed is selected in pelletizing in the S2.
The performance parameter of the embodiment 1-3 fire-retardant enhancing PA6/PBT material of high CTI high-impact being prepared is carried out respectively
Detection, and compared with the existing common high fire-retardant enhancing PA6/PBT material of CTI high-impact, test result is as follows shown in table:
It is by data comparison data in table it is found that enhancing PA6/ more fire-retardant than the high CTI high-impact prepared by optimization formula
The indexs such as impact strength, CTI value and the flame retardant property of PBT material are substantially better than existing common high CTI high-impact on the market
Fire-retardant enhancing PA6/PBT material, especially in 30 parts of PA6,20 parts of PBT, 30 parts of glass fibre, 15 parts of composite flame-proof master batch, phase
Hold 3 parts of toughener, 0.8 part of antioxidant, 1.2 parts of lubricant, meanwhile, it is by the condition mixed in S1 control during the preparation process
800r/min, mixing time 5-10min, and double screw extruder diameter is less than 120mm in S3, twin-screw extrusion machine host turns
Number 300-500r/min, barrel temperature are 240-270 DEG C, 20-50 DEG C of sink temperature, and pelleter revolving speed is selected in pelletizing in the S2
When for 400-700r/min, impact strength, the CTI value of the prepared fire-retardant enhancing PA6/PBT material of high CTI high-impact come out
And the indexs such as flame retardant property can be optimal value.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (7)
1. a kind of fire-retardant enhancing PA6/PBT material of high CTI high-impact, it is characterised in that: it is described to prepare raw material according to the mass fraction,
Including following component: 10-45 parts of PA6,10-45 parts of PBT, 10-30 parts of glass fibre, 10-20 parts of composite flame-proof master batch, compatible
1-5 parts of toughener, 0.2-1.5 parts of antioxidant, 0.2-2.0 parts of lubricant；
The PA6 is polycaprolactam；
The PBT is polybutylene terephthalate (PBT)；
The composite flame-proof master batch is the mixture of iron red phosphorus master batch 40, melamine polyphosphate 30 and high CTI auxiliary agent 20；
The compatible toughening agents are maleic anhydride grafted ethene octene copolymer；
The glass fibre includes long glass fibres and short glass fiber, the diameter of the long glass fibres and short glass fiber
It is 8-15 μm；
The antioxidant includes four (3,5- di-t-butyl -4- hydroxyl) benzenpropanoic acid pentaerythritol esters, and three (2,4- di-t-butyl) are sub-
Phenyl phosphate, N, N '-bis--(3- (3,5- di-tert-butyl-hydroxy phenyl) propiono) hexamethylene diamine；
The lubricant is polyethylene wax, EBS, silicone, silicone oil and combinations thereof.
2. a kind of high fire-retardant enhancing PA6/PBT material of CTI high-impact according to claim 1, it is characterised in that: the horse
The grafting rate of maleic anhydride grafted ethylene octene copolymer is 1.5%.
3. a kind of high fire-retardant enhancing PA6/PBT material of CTI high-impact according to claim 1, it is characterised in that: the glass
The modified glass-fiber that glass fiber is selected.
4. a kind of high fire-retardant enhancing PA6/PBT material of CTI high-impact according to claim 1, it is characterised in that: the system
The each component mass parts of standby raw material are respectively 20-40 parts of PA6,10-30 parts of PBT, 15-30 parts of glass fibre, composite flame-proof mother
Grain 10-20 parts, 1-5 parts of compatible toughening agents, 0.2-1.5 parts of antioxidant, 0.2-2.0 parts of lubricant.
5. a kind of high fire-retardant enhancing PA6/PBT material of CTI high-impact according to any one of claims 1-4, provides one kind
The preparation method of the high fire-retardant enhancing PA6/PBT material of CTI high-impact, specifically includes following operating procedure:
S1: raw material premix are closed: by the proportion by weight of above-mentioned raw materials, take it is dry after PA6, PBT and compatible toughening agents, and by its
It is placed in high-speed mixer together with antioxidant and lubricant, is sufficiently mixed at normal temperature uniformly, obtains mixture, it is spare；
S2: the modification of glass fibre:
(1) glass fibre is placed in working gas is nitrogen, and operating pressure 10-20Pa, discharge power is the low temperature of 80-110W
100-120s is handled in plasma device, obtains pretreated glass fiber；
(2) methacrylic acid and water are mixed by solid-to-liquid ratio (2-6) g:100mL, is turned at 80-90 DEG C with 200-400r/min
Speed stirring 20-40min, obtains methacrylic acid solution；
(3) pretreated glass fiber and methacrylic acid solution are mixed by solid-to-liquid ratio (8-12) g:100mL, at 80-90 DEG C
40-60min is stirred with the revolving speed of 200-400r/min, obtained solid is dried in vacuo 12-18h at 80-90 DEG C, to obtain
Modified glass-fiber；
S3: mixture obtained in S1 is added in the double screw extruder from the main spout of double screw extruder, meanwhile,
By the proportion by weight of above-mentioned raw materials, the modified glass-fiber prepared in S2 and composite flame-proof master batch are successively squeezed from twin-screw
The side spout of machine is added in the double screw extruder out, and is uniformly mixed in double screw extruder, and pelletizing is then squeezed out
Obtain the fire-retardant enhancing PA6/PBT material of high CTI high-impact.
6. a kind of preparation method of high fire-retardant enhancing PA6/PBT material of CTI high-impact according to claim 5, feature
Be: the condition mixed in the S1 is 800r/min, mixing time 5-10min.
7. a kind of preparation method of high fire-retardant enhancing PA6/PBT material of CTI high-impact according to claim 5, feature
Be: double screw extruder diameter is less than 120mm, twin-screw extrusion machine host revolution 300-500r/min, machine barrel in the S3
Temperature is 240-270 DEG C, 20-50 DEG C of sink temperature, and it is 400-700r/min that pelleter revolving speed is selected in pelletizing in the S2.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| BE1027292B1 (en) * | 2019-10-09 | 2021-08-31 | Energy Res Inst Shandong Academy Sciences | Glass fiber reinforced nylon composite material and method of preparation and applications |
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