CN101608022B - Preparation method of fiber glass reinforced halogen-free flame retardant PBT composition and product thereof - Google Patents
Preparation method of fiber glass reinforced halogen-free flame retardant PBT composition and product thereof Download PDFInfo
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Abstract
The invention provides a preparation method of a fiber glass reinforced halogen-free flame retardant PBT composition, which comprises the following steps of: (1) weighing raw materials of all components by weight percent; (2) treating PBT resin and a composite halogen-free flame retardant raw material; (3) mixing by two steps, including firstly high-speed mixing and then low-speed mixing; (4) using a single screw extrusion machine for extruding and pelletizing; and (5) obtaining products. The invention also discloses a product produced by the method, which comprises the following components by weight percent: 30-70% of polybutylene terephthalate (PBT), 15-25% of composite halogen-free flame retardant, 10-40% of alkali-free short glass fiber, 0.5-5% of flexibilizer, 0.1-0.3% of main antioxidant, 0.1-0.5% of auxiliary antioxidant and 0.1-1% of lubricant. The product has high flame retardance, strength and liquidity, as well as low shrinkage ratio and convenient recovery, and is halogen-free, green and environment protective; therefore, the product is suitable for being used as materials of a computer connector and a radiator, and can be used in industrialized production.
Description
Technical field
The present invention relates to polymeric material field, be specifically related to a kind of high strength that computer connector and scatterer use, high workability, low-shrinkage fiber glass reinforced halogen-free flame retardant PBT composition and preparation method thereof of can be used for.
Background technology
Polybutylene terephthalate, English name polybutylece terephthalate (being called for short PBT), belong to polyester series, be to form, and the oyster white of making via mixing program is translucent to opaque, crystalline thermoplastic polyester's resin by 1.4-butyleneglycol (1.4-Butylene glycol) and terephthalic acid (PTA) or terephthalate (DMT) polycondensation.Have good processability, the fast good moldability of crystallization velocity, thermotolerance height, good weatherability, under wet environment the good characteristics of electric insulating quality retentivity, be specially adapted to the manufacturing of complexity, thin-walled electrical and electronic component.But problems such as that pure PBT exists is inflammable, molding shrinkage is big must be carried out modification and be solved.
At present, the improved method of PBT is mainly reached the purpose of fire-retardant enhancing modified by the method for adding glass enhancing and bromide/ANTIMONY TRIOXIDE SB 203 99.8 PCT.Number of patent application provides a kind of flame-retardant reinforced PBT composition for CN101469106A, in the use that to a certain degree reduces halogen, and can be used as some electrical part materials.With the day by day raising of people to safety and environmental requirement, bromide and ANTIMONY TRIOXIDE SB 203 99.8 PCT flame-retardant system toxicity are big, when burning, can produce a large amount of poisonous irritant gass, unfavorable to personnel escape and rescue, there are Polybrominated biphenyl and Poly Brominated Diphenyl Ethers to discharge when production, use and offal treatment, harm environment and health.Behind the ROHS and two instructions of WEEE announcement in 2003 along with European Union, the respective green environmental regulation is also carried out and implemented in various countries.Each big electronics manufacturer has been put into effect oneself non-halogen plan respectively as apple, SONY, Dell, Hewlett-Packard etc.In the case, fiber glass reinforced halogen-free flame retardant PBT is the inevitable direction of development.
The development trend of the miniaturization of computer components such as computer connector and scatterer, thin-walled property and precise treatment has proposed the market demands of high strength, high workability, low-shrinkage to fiber glass reinforced halogen-free flame retardant PBT.
Summary of the invention
The technical problem to be solved in the present invention is, at present fiber glass reinforced halogen-free flame retardant PBT processing difficulties, intensity is low, product is problem of unstable in injection moulding process, provide a kind of can suitability for industrialized production and use, and the fiber glass reinforced halogen-free flame retardant PBT of the requirement of the high strength that satisfies computer connector and radiator material that can conveniently reclaim, high workability.
For solving the problems of the technologies described above, the present invention realizes by following technical scheme:
A kind of preparation method of fiber glass reinforced halogen-free flame retardant PBT composition, it comprises the steps
(1) weighing: take by weighing each component raw material by weight percentage;
(2) raw material is handled in earlier stage: handle PBT resin and composite halogen-free fire retardant raw material;
(3) mix in two steps: afterwards composite halogen-free fire retardant, toughner, primary antioxidant, auxiliary antioxidant and lubricant were put into the high-speed mixer mixing 3-5 minute will to comprise dried PBT resin, processing, add the non-alkali glass staple fibre, low speed mixing 0.5-1 minute;
(4) extruding pelletization goes out product: the material after will mixing carries out extruding pelletization on Φ 120 single screw extrusion machines, obtain the finished product.
The preparation method of aforesaid fiber glass reinforced halogen-free flame retardant PBT composition, described step (2) also comprises:
(a) it is predrying the PBT resin to be carried out hot air circulation, and bed thickness is lower than 30 millimeters, 120 ℃ dry 4 hours down, moisture content is controlled at below 0.02%;
(b) handle the composite halogen-free fire retardant: take by weighing the A phosphonate according to prescription, according to phosphonate: the ratio of 3% hydrogen peroxide=1: 1-3 was ground 1-2 hour after soaking 2-8 hour, dried; Add high-speed mixer according to the A and the B that will fill a prescription after drying, high-speed mixing 1-3 minute, the γ-An Bingjisanyiyangjiguiwan that adds A and B weight 0.2-0.6% under stirring at low speed carries out surperficial coupling processing then, after the adding high-speed stirring 1-3 minute again, under stirring at low speed, add C then, stirring at low speed 1-2 minute, the composite halogen-free fire retardant after obtaining handling.
The preparation method of aforesaid fiber glass reinforced halogen-free flame retardant PBT composition, described step (4) also comprises, the Heating temperature of single screw extrusion machine is: a district 205-215 ℃, two district 215-225 ℃, three district 220-230 ℃, four district 225-235 ℃, five district 230-240 ℃, six district 225-235 ℃, die head 220-230 ℃; Screw speed: 40-150 rev/min.
Adopt the fiber glass reinforced halogen-free flame retardant PBT composition of method for preparing, it comprises the component of following weight part ratio: polybutylene terephthalate (PBT) 30～70%; Composite halogen-free fire retardant 15～25%; Non-alkali glass staple fibre 10～40%; Toughner 0.5～5%; Primary antioxidant 0.1～0.3%; Auxiliary antioxidant 0.1～0.5%; Lubricant 0.1～1%.
Aforesaid fiber glass reinforced halogen-free flame retardant PBT composition also comprises described polybutylene terephthalate limiting viscosity [η]=0.9 ~ 1.20dl/g.
Aforesaid fiber glass reinforced halogen-free flame retardant PBT composition, also comprise described composite halogen-free fire retardant by: A, B, three kinds of components of C are formed, three's weight part ratio is: A60～98%, B0～30%, C0～10%, wherein the A component is handled one or more phosphonates for process, and B is one or more melamine salts, and C is the superpolymer silicone powder that contains siloxanes group.Its preferred proportion of composite halogen-free fire retardant is: A70～96%, B2～20%, C1～6%.
Aforesaid fiber glass reinforced halogen-free flame retardant PBT composition comprises that also described alkali free glass fibre is the short fiber of the silane coupling agent processing of length 8-20 millimeter.
Aforesaid fiber glass reinforced halogen-free flame retardant PBT composition comprises that also described toughner is the SEBS of maleic anhydride graft, and percentage of grafting is 0.2～1%.
Aforesaid fiber glass reinforced halogen-free flame retardant PBT composition comprises that also described primary antioxidant is four (β-(3,5-di-t-butyl 4-hydroxy phenyl) propionic acid) pentaerythritol ester, antioxidant 1010; Auxiliary antioxidant is three (2, the 4-di-t-butyl) phenyl-phosphite, oxidation inhibitor 168; Lubricant is partly-hydrolysed illiteracy dawn ester type waxes.
Beneficial effect of the present invention: according to the fiber glass reinforced halogen-free flame retardant PBT composition of technique scheme preparation, owing to have high flame retardant, high strength, high workability, low-shrinkage, so can be used as the electrical equipment instrument of especially miniaturization of material, thin-walled property and the precise treatment of computer connector and scatterer, and it reclaims conveniently, halogen, environmental protection meets the requirement that country advocates the development green material.
Below in conjunction with drawings and Examples to further instruction of the present invention.
Description of drawings
Fig. 1 is the preparation method's of the embodiment of the invention 1 fiber glass reinforced halogen-free flame retardant PBT composition a process flow diagram.
Embodiment
Embodiment 1: this embodiment provides a kind of preparation method of fiber glass reinforced halogen-free flame retardant PBT composition, and it comprises the steps:
(1) takes by weighing raw material: take by weighing each component raw material by weight percentage;
(2) raw material is handled in earlier stage
(a) processing of PBT resin: it is predrying that the limiting viscosity of PBT resin [η]=1.10 ± 0.01dl/g, PBT resin are carried out hot air circulation earlier, and bed thickness is lower than 30 millimeters, and 120 ℃ were descended dry 4 hours, moisture content is controlled at below 0.02%.
(b) processing of composite halogen-free fire retardant raw material
Composite halogen-free fire retardant three part by weight is A: B: C=93: 5: 2.
1. take by weighing the A phosphonate according to prescription, according to phosphonate: the ratio of 3% hydrogen peroxide=1: 1-3 was soaked after 2-8 hour, ground 1-2 hour, dried;
2. A and B after will drying according to prescription add high-speed mixer, high-speed mixing 1-3 minute, the γ-An Bingjisanyiyangjiguiwan that adds A and B weight 0.2-0.6% under stirring at low speed carries out surperficial coupling processing then, after the adding high-speed stirring 1-3 minute again, under stirring at low speed, add C then, stirring at low speed 1-2 minute, the composite halogen-free fire retardant after obtaining handling.
(3) mix in two steps: afterwards composite halogen-free fire retardant, toughner, primary antioxidant, auxiliary antioxidant and lubricant are put into high-speed mixer mixing 4 minutes at first will to comprise dried PBT resin, processing, add the non-alkali glass staple fibre then, low speed mixing 45 seconds obtains compound;
(4) single screw extrusion machine extruding pelletization: the material after will mixing carries out extruding pelletization on Φ 120 single screw extrusion machines, single screw extrusion machine is respectively distinguished temperature and is set at: a district 205-215 ℃, two district 215-225 ℃, three district 220-230 ℃, four district 225-235 ℃, five district 230-240 ℃, six district 225-235 ℃, die head 220-230 ℃.Screw speed: 80-120 rev/min.
(5) go out product.
The fiber glass reinforced halogen-free flame retardant PBT composition that adopts aforesaid method to make, it comprises following component by weight percentage: polybutylene terephthalate 47.2%; Composite halogen-free fire retardant 19%; Non-alkali glass staple fibre 30%; Toughner 3%; Primary antioxidant 0.2%; Auxiliary antioxidant 0.3%; Lubricant 0.3%.
Wherein, used polybutylene terephthalate limiting viscosity is [η]=0.9～1.20dl/g.
Used alkali free glass fibre is that the silane coupling agent of length 8-20 millimeter is handled short fiber.
Used toughner is the SEBS of maleic anhydride graft, and percentage of grafting is 0.2 ~ 1%.
Used primary antioxidant is four (β-(3,5-di-t-butyl 4-hydroxy phenyl) propionic acid) pentaerythritol ester, antioxidant 1010.
Used auxiliary antioxidant is three (2, the 4-di-t-butyl) phenyl-phosphite, oxidation inhibitor 168.
So lubricant be partly-hydrolysed illiteracy dawn ester type waxes.
Embodiment 2: a kind of fiber glass reinforced halogen-free flame retardant PBT composition is provided, its basic technical scheme is identical with embodiment 1, its difference is, this fiber glass reinforced halogen-free flame retardant PBT composition comprises the component of following weight part ratio: polybutylene terephthalate 52.2%; Composite halogen-free fire retardant 19%; Non-alkali glass staple fibre 25%; Toughner 3%; Primary antioxidant 0.2%; Auxiliary antioxidant 0.3%; Lubricant 0.3%.
Embodiment 3: this embodiment provides a kind of fiber glass reinforced halogen-free flame retardant PBT composition, its basic technical scheme is identical with embodiment 1, its difference is that this fiber glass reinforced halogen-free flame retardant PBT composition comprises the component of following weight part ratio: polybutylene terephthalate 42.2%; Composite halogen-free fire retardant 19%; Non-alkali glass staple fibre 35%; Toughner 3%; Primary antioxidant 0.2%; Auxiliary antioxidant 0.3%; Lubricant 0.3%.
Embodiment 4: this embodiment provides a kind of fiber glass reinforced halogen-free flame retardant PBT composition, its basic technical scheme is identical with embodiment 1, its difference is that this fiber glass reinforced halogen-free flame retardant PBT composition comprises the component of following weight part ratio: polybutylene terephthalate 51.2%; Composite halogen-free fire retardant 15%; Non-alkali glass staple fibre 30%; Toughner 3%; Primary antioxidant 0.2%; Auxiliary antioxidant 0.3%; Lubricant 0.3%.
Embodiment 5: this embodiment provides a kind of fiber glass reinforced halogen-free flame retardant PBT composition, its basic technical scheme is identical with embodiment 1, its difference is that this fiber glass reinforced halogen-free flame retardant PBT composition comprises the component of following weight part ratio: polybutylene terephthalate 41.2%; Composite halogen-free fire retardant 25%; Non-alkali glass staple fibre 30%; Toughner 3%; Primary antioxidant 0.2%; Auxiliary antioxidant 0.3%; Lubricant 0.3%.
Embodiment 6: this embodiment provides a kind of fiber glass reinforced halogen-free flame retardant PBT composition, its basic technical scheme is identical with embodiment 1, its difference is, this fiber glass reinforced halogen-free flame retardant PBT composition, it comprises the component of following weight part ratio: polybutylene terephthalate 45.2%; Composite halogen-free fire retardant 19%; Non-alkali glass staple fibre 30%; Toughner 5%; Primary antioxidant 0.2%; Auxiliary antioxidant 0.3%; Lubricant 0.3%.
The comparative example 1: this embodiment of this embodiment provides a kind of fiber glass reinforced halogen-free flame retardant PBT composition, the basic technical scheme of its component that comprises by weight percentage and preparation is identical with embodiment 1, its difference is, the twin screw extruder of Φ 75 is adopted in its preparation methods steps (4) processing, each is distinguished temperature and is set at: a district 210-220 ℃, two district 220-230 ℃, three district 230-240 ℃, four district 230-240 ℃, five district 235-245 ℃, six district 230-240 ℃, die head 225-235 ℃.Screw speed: 250-350 rev/min.
The comparative example 2: this embodiment provides a kind of fiber glass reinforced halogen-free flame retardant PBT composition, the basic technical scheme of its component that comprises by weight percentage and preparation is identical with embodiment 1, its difference is, the limiting viscosity of PBT resin [η]=0.9dl/g.
The salient features test: the particle of producing is made the standard testing batten according to standard, carries out every test.The material property of performance test accepted standard and each embodiment sees Table 1.
| Component title test event | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | The comparative example 1 | The comparative example 1 |
| Mould shrinking percentage % | 0.3 | 0.5 | 0.3 | 0.3 | 0.3 | 0.3 | 0.4 | 0.2 |
| Heat-drawn wire ℃ | 210.5 | 205.3 | 210.7 | 208.6 | 210.4 | 206. 2 | 207.3 | 205.6 |
| Tensile strength kg/mm 2 | 890 | 867 | 921 | 876 | 887 | 849 | 720 | 780 |
| Elongation % | 3.2 | 3.5 | 0.9 | 3.3 | 0.5 | 4.3 | 4.5 | 1.5 |
| Flexural strength kg/cm 2 | 1300 | 1250 | 1410 | 1370 | 1210 | 1240 | 990 | 1080 |
| Notched Izod impact strength Kgfcm/cm | 8.5 | 8.3 | 8.0 | 8.9 | 7.9 | 8.7 | 7.4 | 6.9 |
| Flame retardant resistance | V0 | V0 | V0 | V2 | V0 | V1 | V0 | V0 |
| Oxygen index % | 31.7 | 32 | 31 | 27 | 33 | 29 | 31 | 31 |
| Dielectric strength Kv/mm | ≥22 | ≥22 | ≥22 | ≥22 | ≥22 | ≥22 | ≥22 | ≥22 |
The material property of each embodiment of table 1
The performance test accepted standard: the mould shrinking percentage is pressed the ASTMD-955 test; Heat-drawn wire is pressed the ASTMD-648 test; Tensile strength is pressed the ASTMD-638 test; Elongation is pressed the ASTMD-638 test; Flexural strength is pressed the ASTMD-790 test; Notched Izod impact strength is pressed the ASTMD-256 test; Flame retardant resistance is pressed the UL94 test; Oxygen index is pressed the GB/T2406 test; Dielectric strength is pressed the GB/T1408 test.
Embodiment 1-6 and comparative example 1-2 show that adding toughner is very big to the flame retardant properties influence in system, and the limiting viscosity of PBT is bigger to the influence of physical strength.Working method has tangible influence to performance simultaneously, mainly is that the twin screw shearing resistance is bigger, is unfavorable for the maintenance of glass fibre length.
The present invention is not limited to the foregoing description, identical with the above embodiment of the present invention or the proximate component of every employing, or realize all embodiments of the object of the invention with same or similar method, all within protection scope of the present invention.
Claims (8)
1. the preparation method of a fiber glass reinforced halogen-free flame retardant PBT composition is characterized in that: comprise the steps
(1) raw materials weighing: take by weighing each component raw material by weight percentage;
(2) it is predrying the PBT resin to be carried out hot air circulation, and bed thickness is lower than 30 millimeters, 120 ℃ dry 4 hours down, moisture content is controlled at below 0.02%;
(3) take by weighing the A phosphonate according to prescription, according to phosphonate: the ratio of 3% hydrogen peroxide=1: 1-3 was soaked after 2-8 hour, ground 1-2 hour, dried; Add high-speed mixer according to the A and the B that will fill a prescription after drying, high-speed mixing 1-3 minute, the γ-An Bingjisanyiyangjiguiwan that adds A and B weight 0.2-0.6% under stirring at low speed carries out surperficial coupling processing then, after the adding high-speed stirring 1-3 minute again, under stirring at low speed, add C then, stirring at low speed 1-2 minute, composite halogen-free fire retardant after obtaining handling, wherein the A component is handled one or more phosphonates for process, the B component is one or more melamine salts, and the C component is the superpolymer silicone powder that contains siloxanes group, and three's weight part ratio is: A60～98%, B0～30%, C0～10%;
(4) afterwards composite halogen-free fire retardant, toughner, primary antioxidant, auxiliary antioxidant and lubricant were put into the high-speed mixer mixing 3-5 minute, adding non-alkali glass staple fibre, low speed mixing 0.5-1 minute will to comprise dried PBT resin, processing;
(5) extruding pelletization goes out product: the material after will mixing carries out extruding pelletization on single screw extrusion machine, obtain goods.
2. the preparation method of fiber glass reinforced halogen-free flame retardant PBT composition according to claim 1, it is characterized in that: described step (5) also comprises, the single screw extrusion machine Heating temperature is: a district 205-215 ℃, two district 215-225 ℃, three district 220-230 ℃, four district 225-235 ℃, five district 230-240 ℃, six district 225-235 ℃, die head 220-2300; Screw speed: 40-150 rev/min.
3. the preparation method of fiber glass reinforced halogen-free flame retardant PBT composition according to claim 1, it is characterized in that: described step (5) comprises that also the specification of single screw extrusion machine is Φ 120.
4. a fiber glass reinforced halogen-free flame retardant PBT composition that adopts the described method preparation of claim 1 is characterized in that: the component that comprises following weight part ratio: polybutylene terephthalate (PBT) 30～70%; Composite halogen-free fire retardant 15～25%; Non-alkali glass staple fibre 10～40%; Toughner 0.5～5%; Primary antioxidant 0.1～0.3%; Auxiliary antioxidant 0.1～0.5%; Lubricant 0.1～1%; Described composite halogen-free fire retardant is made up of A, B, three kinds of components of C, three's weight part ratio is: A60～98%, B0～30%, C0～10%, wherein the A component is handled one or more phosphonates for process, the B component is one or more melamine salts, and the C component is the superpolymer silicone powder that contains siloxanes group.
5. fiber glass reinforced halogen-free flame retardant PBT composition according to claim 4 is characterized in that: described polybutylene terephthalate limiting viscosity [η]=0.9～1.20dl/g.
6. fiber glass reinforced halogen-free flame retardant PBT composition according to claim 4 is characterized in that: alkali free glass fibre is the short fiber that the silane coupling agent of length 8-20 millimeter is handled.
7. fiber glass reinforced halogen-free flame retardant PBT composition according to claim 4 is characterized in that: toughner is the SEBS of maleic anhydride graft, and percentage of grafting is 0.2～1%.
8. fiber glass reinforced halogen-free flame retardant PBT composition according to claim 4 is characterized in that: primary antioxidant is four (β-(3,5-di-t-butyl 4-hydroxy phenyl) propionic acid) pentaerythritol ester; Auxiliary antioxidant is three (2, the 4-di-t-butyl) phenyl-phosphite; Lubricant is partly-hydrolysed illiteracy dawn ester type waxes.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101817972A (en) * | 2010-04-28 | 2010-09-01 | 深圳市科聚新材料有限公司 | Flame-retardant enhanced PBT material and preparation method thereof |
| CN102786779A (en) * | 2011-05-16 | 2012-11-21 | 山东道恩高分子材料股份有限公司 | High-impact glass fiber reinforced halogen-free flame retardation PBT material |
| CN102848485B (en) * | 2012-08-31 | 2014-10-08 | 华南理工大学 | Method for recovery and granulation of high performance glass fiber reinforced liquid crystalline polymer secondary material |
| CN103965593A (en) * | 2014-03-31 | 2014-08-06 | 东莞市美塑塑料科技有限公司 | Preparation method of high-strength glass-fiber-reinforced halogen-free flame-retardant PBT (polybutylene terephthalate) |
| CN106750111A (en) * | 2016-12-27 | 2017-05-31 | 安徽潜源教学设备有限公司 | A kind of polyurethane plastic runway of glass fiber reinforcement and preparation method thereof |
| CN109535664B (en) * | 2018-10-30 | 2020-12-01 | 惠州市中海源新材料科技有限公司 | High polymer material for connector |
| CN112724616A (en) * | 2020-12-22 | 2021-04-30 | 江阴济化新材料有限公司 | Halogen-free flame-retardant PBT (polybutylene terephthalate) material and preparation process thereof |
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