CN103044912B - Halogen-free flameproof continuous long glass fiber reinforced polyamide 66 composite material and preparation method thereof - Google Patents
Halogen-free flameproof continuous long glass fiber reinforced polyamide 66 composite material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of halogen-free flameproof continuous long glass fiber reinforced polyamide 66 composite material, be made up of following each component based on total weight percent: polyamide 66 42 ~ 72.5%, toughener 2 ~ 6%, halogen-free flame retardants 10 ~ 20%, heat stabilizer 0.5 ~ 2.0% and long glass fibres 15 ~ 30%；The relative viscosity of wherein said polyamide 66 is 2.0 ~ 3.0；Described long glass fibres is polyamide 66 special LFT alkali-free continuous long glass fiber.The present invention prepares the material of gained and has high fluidity, excellent thermostability, high rigidity, HI high impact, high-dimensional stability, excellent fire resistance and high CTI value, its hot strength >=150MPa, bending modulus >=7000MPa, notch impact strength >=15KJ/m after testing2, heat distortion temperature (1.80MPa) >=250 DEG C, flame retardant rating reaches UL94 1.6mmV 0, CTI value >=500V, and the present invention uses the shortcoming that the technology of high/low temperature double melt immersion slot series connection solves halogen-free flame retardants pyrolytic.
Description
Technical field
The present invention relates to a kind of halogen-free flame-retardant polymer composite, particularly relate to one
Halogen-free flame-retardant long fiber glass reinforced polyamide 66 composite and preparation method thereof.
Background technology
Fiber glass reinforced polyamide 66 product has excellent integrated application performance, extensively
It is applied to the fields such as electric.Along with the raising day by day of entire society's environmental consciousness,
Halogen-free flameproof becomes the main flow of fiber glass reinforced polyamide 66 technology development.But glass increases
Strong polyamide 66 V-0 to be reached grade non-halogen flame-retardant needs to add a lot of halogen-free flame retardants,
This meeting seriously reduces the mechanical property of the material of fiber glass reinforced polyamide 66, particularly
Notch impact strength.If the enhancing glass of halogen-free flame-retardant polyamide 66 uses the longest
Glass fibre improves to obtain long glass fiber reinforced polyamide 66 (LFTPA66), then Halogen resistance
The mechanical property of retardant polyamide 66 will General Promotion, just can realize its high-performance
Change, but due in LFTPA66 production process for ensureing that polyamide 66 is to continuously long
The effect of impregnation of glass fibre, the melt temperature of polyamide 66 is generally arranged very
High (>=300 DEG C), and under high temperature, halogen-free flame retardants can decompose severe decomposition.
Summary of the invention
In order to overcome above-mentioned the deficiencies in the prior art, the invention provides one
Halogen-free flameproof continuous long glass fiber reinforced polyamide 66 composite material and preparation method thereof,
This composite, by using continuous long glass fiber reinforced, makes halogen-free flame-retardant polyamide 66
High performance, and improve existing preparation technology, solve Halogen in impregnation process
The shortcoming of fire retardant pyrolytic.
The present invention is to solve that its technical problem be the technical scheme is that
A kind of halogen-free flameproof continuous long glass fiber reinforced polyamide 66 composite material, by with
Under based on total weight percent each component composition:
The relative viscosity of wherein said polyamide 66 is 2.0～3.0；Described long glass fibers
Dimension is polyamide 66 special LFT alkali-free continuous long glass fiber.
Its further technical scheme is:
Described heat stabilizer is acryloyl group functional group and the compound species of monothioester, Asia
At least one in phosphoric acid ester, half Hinered phenols, amine and calixarenes.
Described toughener is polar monomer graft polymer, and wherein polymer is poly-second
Alkene, polypropylene, ethylene-α-ethylene-octene copolymer, styrene are total to butadiene
Polymers, polyethylene-polystyrene-polypropylene terpolymer, ethylene-propylene-fourth two
Alkene terpolymer, ethylene-vinyl acetate copolymer, ethylene-acrylate copolymers
In thing and ethylene-acrylate-glycidyl methacrylate copolymer at least
A kind of；Described polar monomer is can the anhydrides monomer of double-bond polymerization, acrylic compounds list
At least one in body and acrylic ester monomer.
Described can the anhydrides monomer of double-bond polymerization be maleic anhydride, citraconic anhydride and second
At least one in enetutanedioic acid anhydride；Described acrylic monomer is acrylic acid and first
At least one in base acrylic acid；Described acrylic ester monomer be acrylic acid methyl ester.,
In ethyl acrylate, methyl methacrylate and glytidyl methacrylate at least
A kind of.
Described halogen-free flame retardants is organic hypophosphites, melamine polyphosphate and three
At least one in poly cyanamid cyanurate.
Present invention also offers a kind of halogen-free flameproof continuous long glass fiber reinforced polyamide 66
The preparation method of composite, comprises the following steps:
(1) Single screw extrusion is passed through by the 20～50wt.% of described polyamide 66 total amount
Being transported to high-temperature fusant immersion slot by mouth die after machine plasticizing, described high-temperature fusant infiltrates
In groove, temperature is 320～380 DEG C, and described high-temperature fusant immersion slot is a length of
2～2.5m；
(2) thermally-stabilised by remaining polyamide 66,0.5～2.0wt.% described in (1)
Agent, 2～6wt.% toughener and 10～20wt.% halogen-free flame retardants pass through Single screw extrusion
Being transported to low-temperature melt immersion slot by mouth die after machine plasticizing, described low-temperature melt infiltrates
In the groove of groove, temperature is 275～290 DEG C, and described low-temperature melt immersion slot is a length of
1～1.5m；
(3) 15～30wt.% long glass fibres are led with the speed of 25～70m/min
Draw the low-temperature melt leaching in the high-temperature fusant immersion slot and (2) sequentially entered in (1)
Profit groove, after being infiltrated by traction and cooled down, uses the special pelleter of LFT to cut into
The long particle of 12mm.
The method have the benefit that: the present invention is increased by continuous long glass fiber
Force halogen-free flame-retardant polyamide high performance, use high and low temperature melt immersion slot simultaneously
The production technology of series connection, realizes first achievement unit segregation acyl in high-temperature fusant immersion slot
The infiltration to long glass fibres of amine 66 resin, then in low-temperature melt in immersion slot
Being coated with one layer of polyamide 66 and add the outer layer of halogen-free flame retardants, final product is internal layer
It is polyamide 66 and Halogen for polyamide 66 infiltration long glass fibres master batch, outer layer
The complex of fire retardant, ectonexine can realize fully dividing in later product injection moulding process
Dissipating, this technology can effectively solve polyamide 66 halogen-free flameproof under the condition of high temperature
Serious defect, products obtained therefrom hot strength >=150MPa, bending modulus are decomposed in agent
>=7000MPa, notch impact strength >=15KJ/m2, heat distortion temperature (1.80MPa)
>=250 DEG C, flame retardant rating reaches UL94 1.6mmV-0, CTI value >=500V.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in further detail, but this
Invention is not limited to following embodiment.
Embodiment one:
The first step: by 15 kilograms of polyamide 66 153HSL by draw ratio 20:1
It is transported to high-temperature fusant immersion slot, described height by mouth die after single screw extrusion machine plasticizing
In the groove of temperature melt immersion slot, temperature is 320 DEG C, and described high-temperature fusant infiltration flute length
Degree is 2m；
Second step: by 57.5 kilograms of polyamide 66 153HSL, 2 kilograms of toughener
493D, 1010,0.3 kilogram of phosphite antioxidant of 0.2 kilogram of phenolic thermostabilizers
168,10 kilograms of Ke Laien fire retardant OP 1312 are by the mono-screw rod of draw ratio 20:1
It is transported to low-temperature melt immersion slot, described low-temperature melt by mouth die after extruder plasticizing
In the groove of immersion slot, temperature is 275 DEG C, and described low-temperature melt immersion slot is a length of
1m；
3rd step: 15 kilograms of PPG companies are produced continuous long glass fiber Tufrov
4510 sequentially pass through the high-temperature fusant groove in the first step and with 25mm/min speed
Low-temperature melt groove in two steps, after long glass fibres draws infiltration from melt tank, uses
The special pelleter of LFT is cut into the particle that 12mm length is homogeneous, obtains composite A, its
Performance is as shown in table 1:
The performance of table 1 composite A
| Performance | Unit | Testing standard | Test result |
| Density (23 DEG C) | g/cm3 | ISO 1183 | 1.32 |
| Glass fiber content (750 DEG C, 30min) | % | ISO 3451/1 | 15 |
| HDT(1.80MPa) | ℃ | ISO75/1-93 | 251 |
| Hot strength | MPa | ISO527/2-93 | 155 |
| Bending modulus | MPa | ISO178/2-93 | 7200 |
| Notch impact strength | KJ/m2 | ISO179/2-93 | 17.5 |
| Anti-flammability | -- | UL94 | 1.6mmV-0 |
| CTI value | V | IEC 60112 | 600 |
Embodiment two:
The first step: by 20 kilograms of polyamide 66 71G13L by draw ratio 20:1
It is transported to high-temperature fusant immersion slot, described height by mouth die after single screw extrusion machine plasticizing
In the groove of temperature melt immersion slot, temperature is 340 DEG C, and described high-temperature fusant infiltration flute length
Degree is 2m；
Second step: by 40 kilograms of polyamide 66 71G13L, 4 kilograms of toughener 560D,
1010,0.5 kilogram of phosphite antioxidant 627A of 0.5 kilogram of phenolic thermostabilizers,
15 kilograms of Ke Laien fire retardant OP 1311 are by draw ratio 20:1 Single screw extrusion
Being transported to low-temperature melt immersion slot by mouth die after machine plasticizing, described low-temperature melt infiltrates
In the groove of groove, temperature is 280 DEG C, and the described a length of 1m of low-temperature melt immersion slot；
3rd step: 20 kilograms of PPG companies are produced continuous long glass fiber Tufrov
4510 sequentially pass through the high-temperature fusant groove in the first step and with 50mm/min speed
Low-temperature melt groove in two steps, after long glass fibres draws infiltration from melt tank, uses
The special pelleter of LFT is cut into the particle that 12mm length is homogeneous, obtains composite B, its
Performance is as shown in table 2:
The performance of table 2 composite B
| Performance | Unit | Testing standard | Test result |
| Density (23 DEG C) | g/cm3 | ISO 1183 | 1.39 |
| Glass fiber content (750 DEG C, 30min) | % | ISO 3451/1 | 20 |
| HDT(1.80MPa) | ℃ | ISO75/1-93 | 254 |
| Hot strength | MPa | ISO527/2-93 | 180 |
| Bending modulus | MPa | ISO178/2-93 | 7800 |
| Notch impact strength | KJ/m2 | ISO179/2-93 | 20.0 |
| Anti-flammability | -- | UL94 | 1.6mmV-0 |
| CTI value | V | IEC 60112 | 600 |
Embodiment three:
The first step: by 20 kilograms of polyamide 66 70K20HSL by draw ratio 20:
It is transported to high-temperature fusant immersion slot by mouth die after 1 single screw extrusion machine plasticizing, described
In the groove of high-temperature fusant immersion slot, temperature is 360 DEG C, and described high-temperature fusant immersion slot
A length of 2.5m；
Second step: by 33.5 kilograms of polyamide 66 70K20HSL, 5 kilograms toughness reinforcing
Agent Bondyram 1010,0.7 kilogram of phosphorous of 7003,0.8 kilogram of phenolic thermostabilizers
Acid esters antioxidant 627A, 10 kilograms of Ke Laien fire retardant OP1230 and 5 kilograms of resistances
Combustion agent MPP is defeated by mouth die after being plastified by draw ratio 20:1 single screw extrusion machine
Delivering to low-temperature melt immersion slot, in the groove of described low-temperature melt immersion slot, temperature is
285 DEG C, and the described a length of 1.5m of low-temperature melt immersion slot；
3rd step: 25 kilograms of PPG companies are produced continuous long glass fiber Tufrov
4588 sequentially pass through the high-temperature fusant groove in the first step and with 70mm/min speed
Low-temperature melt groove in two steps, after long glass fibres draws infiltration from melt tank, uses
The special pelleter of LFT is cut into the particle that 12mm length is homogeneous, obtains composite C, its
Performance is as shown in table 3:
The performance of table 3 composite C
| Performance | Unit | Testing standard | Test result |
| Density (23 DEG C) | g/cm3 | ISO 1183 | 1.43 |
| Glass fiber content (750 DEG C, 30min) | % | ISO 3451/1 | 25 |
| HDT(1.80MPa) | ℃ | ISO75/1-93 | 255 |
| Hot strength | MPa | ISO527/2-93 | 195 |
| Bending modulus | MPa | ISO178/2-93 | 8700 |
| Notch impact strength | KJ/m2 | ISO179/2-93 | 23 |
| Anti-flammability | -- | UL94 | 1.6mmV-0 |
| CTI value | V | IEC 60112 | 550 |
Embodiment four:
The first step: 20 kilograms of polyamide 66 101L are mono-by draw ratio 20:1
It is transported to high-temperature fusant immersion slot, described high temperature by mouth die after screw extruder plasticizing
In the groove of melt immersion slot, temperature is 380 DEG C, and described high-temperature fusant immersion slot length
For 2.3m；
Second step: by 22 kilograms of polyamide 66 101L, 6 kilograms of toughener 560D,
1010,1 kilogram of phosphite antioxidant 412S of 1 kilogram of phenolic thermostabilizers, 15
Kilogram Ke Laien fire retardant OP1312 and 5 kilograms of fire retardant MCA passes through draw ratio
It is transported to low-temperature melt immersion slot by mouth die after the plasticizing of 20:1 single screw extrusion machine,
In the groove of described low-temperature melt immersion slot, temperature is 290 DEG C, and the leaching of described low-temperature melt
Profit slot length is 1.3m；
3rd step: 30 kilograms of PPG companies are produced continuous long glass fiber Tufrov
4588 sequentially pass through the high-temperature fusant groove in the first step and with 70mm/min speed
Low-temperature melt groove in two steps, after long glass fibres draws infiltration from melt tank, uses
The special pelleter of LFT is cut into the particle that 12mm length is homogeneous, obtains composite D, its
Performance is as shown in table 4:
The performance of table 4 composite D
| Performance | Unit | Testing standard | Test result |
| Density (23 DEG C) | g/cm3 | ISO 1183 | 1.47 |
| Glass fiber content (750 DEG C, 30min) | % | ISO 3451/1 | 30 |
| HDT(1.80MPa) | ℃ | ISO75/1-93 | 256 |
| Hot strength | MPa | ISO527/2-93 | 220 |
| Bending modulus | MPa | ISO178/2-93 | 9500 |
| Notch impact strength | KJ/m2 | ISO179/2-93 | 27 |
| Anti-flammability | -- | UL94 | 1.6mmV-0 |
| CTI value | V | IEC 60112 | 500 |
Be can be seen that by above-described embodiment, the present invention prepares the material of gained, and it draws after testing
Stretch intensity >=150MPa, bending modulus >=7000MPa, notch impact strength >=
15KJ/m2, heat distortion temperature (1.80MPa) >=250 DEG C, flame retardant rating reaches
UL94 1.6mmV-0, CTI value >=500V.It has high fluidity, and excellent is resistance to
Hot, high rigidity, HI high impact, high-dimensional stability, excellent fire resistance and
High CTI value, and the present invention uses the technology solution of high/low temperature double melt immersion slot series connection
Determine the shortcoming of halogen-free flame retardants pyrolytic.
Above example is only the exemplary embodiment of the present invention, is not used in and limits this
Bright.Those skilled in the art can be in the essence of the present invention and protection domain, to this
Various amendment or equivalent are made in invention, and this amendment or equivalent also should be regarded as
It is within the scope of the present invention.
Claims (5)
1. the preparation method of a halogen-free flameproof continuous long glass fiber reinforced polyamide 66 composite material, it is characterised in that: comprise the following steps:
(1) it is transported to high-temperature fusant immersion slot by mouth die after being plastified the 20～50wt.% of polyamide 66 formula consumption total amount by single screw extrusion machine, in described high-temperature fusant immersion slot, temperature is 320～380 DEG C, and described high-temperature fusant immersion slot a length of 2～2.5m；
(2) it is transported to low-temperature melt immersion slot by remaining described in (1) after polyamide 66, formula consumption heat stabilizer, formula consumption toughener and formula consumption halogen-free flame retardants are plastified by single screw extrusion machine by mouth die, in the groove of described low-temperature melt immersion slot, temperature is 275～290 DEG C, and described low-temperature melt immersion slot a length of 1～1.5m；
(3) formula consumption long glass fibres is sequentially entered the high-temperature fusant immersion slot in (1) and the low-temperature melt immersion slot in (2) with the speed drawing of 25～70m/min; after infiltrating by traction and cool down, the special pelleter of LFT is used to cut into the long particle of 12mm；
Wherein said halogen-free flameproof continuous long glass fiber reinforced polyamide 66 composite material is made up of following each component based on total weight percent:
The relative viscosity of wherein said polyamide 66 is 2.0～3.0；Described long glass fibres is polyamide 66 special LFT alkali-free continuous long glass fiber.
The preparation method of halogen-free flameproof the most according to claim 1 continuous long glass fiber reinforced polyamide 66 composite material, it is characterised in that: described heat stabilizer is acryloyl group functional group and at least one in the compound species of monothioester, phosphorous acid esters, half Hinered phenols, amine and calixarenes.
The preparation method of halogen-free flameproof the most according to claim 1 continuous long glass fiber reinforced polyamide 66 composite material, it is characterized in that: described toughener is polar monomer graft polymer, wherein polymer is polyethylene, polypropylene, ethylene-α-ethylene-octene copolymer, styrene and the copolymer of butadiene, polyethylene-polystyrene-polypropylene terpolymer, ethylene-propylene-diene terpolymer, ethylene-vinyl acetate copolymer, at least one in vinyl-acrylate copolymer and ethylene-acrylate-glycidyl methacrylate copolymer；Described polar monomer is can at least one in anhydrides monomer, acrylic monomer and the acrylic ester monomer of double-bond polymerization.
The preparation method of halogen-free flameproof the most according to claim 3 continuous long glass fiber reinforced polyamide 66 composite material, it is characterised in that: described can the anhydrides monomer of double-bond polymerization be at least one in maleic anhydride, citraconic anhydride and vinyl succinic anhydride；Described acrylic monomer is at least one in acrylic acid and methacrylic acid；Described acrylic ester monomer is at least one in acrylic acid methyl ester., ethyl acrylate, methyl methacrylate and glytidyl methacrylate.
The preparation method of halogen-free flameproof the most according to claim 1 continuous long glass fiber reinforced polyamide 66 composite material, it is characterised in that: described halogen-free flame retardants is at least one in organic hypophosphites, melamine polyphosphate and melamine cyanurate.
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