CN105273388A - High-heat-resistance halogen-free flame-retardant polyphenyl ether composite material and preparation method thereof - Google Patents
High-heat-resistance halogen-free flame-retardant polyphenyl ether composite material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a high-heat-resistance halogen-free flame-retardant polyphenyl ether composite material and a preparation method thereof. The composite material is prepared from, by weight, 30-50% of polyphenyl ether, 15-50% of syndiotactic polystyrener, 10-40% of glass fiber, 1-7% of halogen-free flame retardant, 2-6% of compatilizer, 0.4-1.0% of antioxidant and 0.2-1.0% of lubricant. Halogen-free flame retardant is red phosphorus master batches with impact-resistant polystyrene as carriers. High-heat-resistance syndiotactic polystyreneresin, red phosphorus master batches which are high in phosphorus content and small in influence on heat resistance, and glass fiber are selected to conduct halogen-free flame retardant modification on polyphenyl ether, and the high-heat-resistance halogen-free flame-retardant polyphenyl ether composite material can be obtained. In addition, graft with PPO or sPS as substrates is added to serve as compatilizer, and therefore the anti-impact performance of high-heat-resistance halogen-free flame-retardant polyphenyl ether can be improved.
Description
Technical field
The present invention relates to the technical field of polyphenylene oxide composite material, more particularly, relate to a kind of high heat-resistant halogen-free flame-retardant polyphenylene oxide composite material and preparation method thereof.
Background technology
The relative density of polyphenylene oxide (PPO) is little, there is a series of excellent properties such as loose, the resistance to creep of proof stress, heat-resisting, resistant to hydrolysis, resistance to water vapour, dimensional stability, there is difficult combustion self-extinguishing simultaneously and keep the features such as excellent electric performance in very wide temperature, range of frequency.But, polyphenylene oxide due to the large processing difficulties of melt viscosity, so generally add other resins, as polystyrene (PS), nylon (PA), acrylonitrile-butadiene-styrene (ABS) (ABS) etc. improve Drawing abillity.But the membership that adds of these resins makes the flame retardant resistance of polyphenylene oxide obviously decline, be not suitable for the field such as electric that flame-retardancy requirements is higher.In order to overcome above shortcoming, people propose various solution, and have applied for Patents.
Chinese patent CN102399433A discloses a kind of for photovoltaic junction box polyphenylene ether composition, its main ingredient comprises: polyphenylene oxide 55 ~ 95 parts, polystyrene 45 ~ 5 parts, toughner 2 ~ 10 parts, phosphate flame retardant 5 ~ 20 parts, said composition has the features such as good flame resistance, heat oxygen aging resistance, excellent electrical properties.Chinese patent CN102702722A discloses a kind of halogen-free flame-proof reinforced poly phenylate/ABS and preparation method thereof, its main ingredient comprises: polyphenylene oxide 10 ~ 50%, ABS10 ~ 40%, Compositional type halogen-free flame retardants 5 ~ 25%, toughner 2 ~ 20%, glass 10 ~ 40%, compatilizer 1 ~ 10%, obtained polyphenylene oxide alloy has the advantages such as good mechanical property, excellent outward appearance, high-impact.Chinese patent CN101570631A discloses a kind of high heat-resisting, halogen-free fire-retardant polyphenyl ether/polystyrene complex and preparation method thereof, this mixture comprises polyphenylene oxide resin, polystyrene, toughner, halogen-free flame retardants and processing aid, wherein, halogen-free flame retardants is one or more the composite uses in micro encapsulation encapsulated red phosphorus and phosphoric acid ester or phosphorous acid ester, and obtained material has heat-resisting height, fire retardant and not easily separates out and the feature such as not halogen-containing.Chinese patent CN102643526A discloses a kind of superelevation thermotolerance halogen-free fire-retardant polyphenyl ether composition, and its main ingredient comprises: polyphenylene oxide 70 ~ 90%, polyphenylene sulfide 0.5 ~ 10%, polystyrene 2 ~ 25%, phosphoric acid ester 1 ~ 10%.Thermotolerance and the mobility of composition is improved by adding polyphenylene sulfide.
Although more than invention provides some useful guidance in the flame retardant resistance improving polyphenylene oxide composite material and thermotolerance, but still comes with some shortcomings: the adding of resin such as (1) acrylonitrile-butadiene-styrene (ABS) (ABS) and polystyrene (PS) make the thermotolerance of polyphenylene oxide significantly decline; (2) phosphate ester flame retardants add the Halogen demand for development meeting environmental protection, but due to very strong plastification, while improving fire retardant, make the thermotolerance of polyphenylene oxide composite material obviously decline; (3) although polyphenylene sulfide can not make the thermotolerance of polyphenylene oxide decline, itself and polyphenylene oxide poor compatibility, affect the mechanical property of material.
Summary of the invention
The object of the invention is to overcome above-mentioned defect of the prior art, a kind of high heat-resistant halogen-free flame-retardant polyphenylene oxide composite material and preparation method thereof is provided.
For achieving the above object, a first aspect of the present invention provides a kind of high heat-resistant halogen-free flame-retardant polyphenylene oxide composite material, and this matrix material is made up of following component by weight percentage:
As preferably, the intrinsic viscosity that described polyphenylene oxide measures in 25 DEG C of chloroforms is 0.35 ~ 0.65dL/g.Polyphenylene oxide molecular weight lower than 0.35dL/g (25 DEG C of chloroforms) is too low, and flame retardant properties is poor, and higher than 0.65dL/g (25 DEG C of chloroforms) although time polyphenylene oxide flame retardant properties good, due to its poor fluidity, bring processing difficulties on the contrary.
As preferably, described syndiotactic polystyrene is high-impact syndiotactic polystyrene, and its Izod notched impact strength is greater than 10KJ/m
2(ISO180,23 DEG C).
As preferably, described glass fibre is alkali-free glass fiber, and filament diameter is 7 ~ 17 μm, chopped length 3 ~ 24mm.The fiber preparation difficulty that diameter is less than 7 μm, and easily wear and tear in composite processing process, loss of strength is very large; The glass that diameter is greater than 17 μm can affect the combination with resin, affects the performance of matrix material equally.
As preferably, described halogen-free flame retardants is the red phosphor masterbatch that impact resistant polystyrene (HIPS) is carrier.Wherein, described red phosphor masterbatch is be the red phosphor masterbatch that 40% ~ 60%, 500 ~ 1500 object red phosphorus first obtain with impact resistant polystyrene extruding pelletization after stablizer, low-molecular-weight wax are coated again by weight percent.
As preferably, described compatilizer is at least one in polyphenylene oxide grafted maleic anhydride (PPO-g-MAH) or syndiotactic polystyrene grafted maleic anhydride (sPS-g-MAH).PPO or sPS is contained in one end of compatilizer, and the other end contains the MAH reacted with glass surface polar groups, can improve the combination of resin and glass, plays better compatible role.
As preferably, described oxidation inhibitor is the composite antioxidant system of hindered phenol, phosphorous acid ester and acid-acceptor composition.Wherein, described hindered phenol is preferably four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester, described phosphorous acid ester is preferably three [2.4-di-tert-butyl-phenyl] phosphorous acid ester, and described acid-acceptor is preferably zinc oxide (ZnO).
As preferably, described lubricant is pentaerythritol stearate.
A second aspect of the present invention provides a kind of preparation method of the high heat-resistant halogen-free flame-retardant polyphenylene oxide composite material as described in technique scheme, comprises the following steps:
(1) 30% ~ 50% polyphenylene oxide, 15% ~ 50% syndiotactic polystyrene, 1% ~ 7% halogen-free flame retardants, 2% ~ 6% compatilizer, 0.4% ~ 1.0% oxidation inhibitor and 0.2% ~ 1.0% lubricant are joined mixing machine mixing;
(2) the above-mentioned material mixed is put into the main feeding hopper of twin screw extruder, add the glass fibre of 10% ~ 40% at side feeding hopper, by twin screw extruder extruding pelletization, obtained high heat-resistant halogen-free flame-retardant polyphenylene oxide composite material.
As preferably, described mixing time is 3 ~ 5min, and the rotating speed of twin screw extruder is 200 ~ 500r/min, and temperature is 250 ~ 290 DEG C.
Compared with prior art, beneficial effect of the present invention is:
1, select the syndiotactic polystyrene (sPS) of excellent heat resistance and polyphenylene oxide (PPO) compound, the thermotolerance of obtained polyphenylene oxide/syndiotactic polystyrene (PPO/sPS) alloy is far above alloys such as polyphenyl ether/styrene (PPO/PS) and polyphenylene oxide/acrylonitrile-butadiene-styrene (ABS)s (PPO/ABS).
2, adopt red phosphor masterbatch to be fire retardant, under the prerequisite realizing material halogen-free flameproof, avoid traditional phosphoric acid ester halogen-free flame retardants to heat-resisting bad effect, select HIPS to be carrier simultaneously, ensure that consistency.
3, adopt polyphenylene oxide grafted maleic anhydride (PPO-g-MAH) and syndiotactic polystyrene grafted maleic anhydride (sPS-g-MAH) as compatilizer, the interface cohesion of resin and glass fibre can be improved, improve Drawing abillity, improve the mechanical property of material.
4, technique of the present invention is simple, and processing characteristics is good, and obtained halogen-free fire-retardant polyphenyl ether has good mechanical performance, and resistance toheat is good, may be used for flame retardant resistance and the high family's electric car of heat resistant requirements and the field such as electric.
Embodiment
For making the object of the embodiment of the present invention, technical scheme and advantage clearly, be clearly and completely described to the technical scheme in the embodiment of the present invention below, obviously, described embodiment is the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
A kind of high heat-resistant halogen-free flame-retardant polyphenylene oxide composite material, this matrix material is made up of following component by weight percentage: polyphenylene oxide 30% ~ 50%, syndiotactic polystyrene 15% ~ 50%, glass fibre 10% ~ 40%, halogen-free flame retardants 1% ~ 7%, compatilizer 2% ~ 6%, oxidation inhibitor 0.4% ~ 1.0%, lubricant 0.2% ~ 1.0%.
The intrinsic viscosity that described polyphenylene oxide measures in 25 DEG C of chloroforms is 0.35 ~ 0.65dL/g.
Described syndiotactic polystyrene is high-impact syndiotactic polystyrene, and its Izod notched impact strength is greater than 10KJ/m
2.
Described glass fibre is alkali-free glass fiber, and filament diameter is 7 ~ 17 μm, chopped length 3 ~ 24mm.
The red phosphor masterbatch of described halogen-free flame retardants to be impact resistant polystyrene be carrier.Described red phosphor masterbatch is be the red phosphor masterbatch that 40% ~ 60%, 500 ~ 1500 object red phosphorus first obtain with impact resistant polystyrene extruding pelletization after stablizer, low-molecular-weight wax are coated again by weight percent.
Described compatilizer is at least one in polyphenylene oxide grafted maleic anhydride or syndiotactic polystyrene grafted maleic anhydride.
Described oxidation inhibitor is the composite antioxidant system of hindered phenol, phosphorous acid ester and acid-acceptor composition.
Described lubricant is pentaerythritol stearate.
A kind of preparation method of high heat-resistant halogen-free flame-retardant polyphenylene oxide composite material, comprise the following steps: 30% ~ 50% polyphenylene oxide, 15% ~ 50% syndiotactic polystyrene, 1% ~ 7% halogen-free flame retardants, 2% ~ 6% compatilizer, 0.4% ~ 1.0% oxidation inhibitor and 0.2% ~ 1.0% lubricant are joined mixing machine mixing, mixing time is 3 ~ 5min, then the main feeding hopper of twin screw extruder is put into, the glass fibre of 10% ~ 40% is added at side feeding hopper, by twin screw extruder extruding pelletization, obtained high heat-resistant halogen-free flame-retardant polyphenylene oxide composite material.Wherein, the rotating speed of twin screw extruder is 200 ~ 500r/min, and temperature is 250 ~ 290 DEG C.
The embodiment of the present invention and comparative example are all injection molded into the standard batten of test according to standard-required and test.Wherein, vertical combustion is according to UL94 standard, and Izod notched impact strength is according to ISO180 standard, and heat-drawn wire test is according to ISO75-2 standard.
The raw material used in the embodiment of the present invention and comparative example is as follows:
Polyphenylene oxide: LXR040 (intrinsic viscosity 0.40dL/g (25 DEG C of chloroforms)), Lanxing Chemical New Material Co., Ltd..
Syndiotactic polystyrene: XAREC
tMs105 (Izod notched impact strength 20KJ/m
2, ISO180,23 DEG C), Japanese bright dipping (Idemitsu) company.
Impact resistant polystyrene: HIPSPH88, Taiwan Qi Mei company.
Glass ECS306: filament diameter 13 μm, chopped length 3mm, Chongqing Polycomp International Co., Ltd.
Compatilizer: CX-1 (PPO-g-MAH), Japanese bright dipping (Idemitsu) company; 9012PA (sPS-g-MAH), German Bi Ke (BYK) company.
Halogen-free flame retardants: REDNIC30450N3 (red phosphor masterbatch, red phosphorus content 50%, HIPS carrier); WSFR-PX-220 (oligomeric aryl phosphate ester), Zhejiang Wansheng Co., Ltd..
Oxidation inhibitor: hindered phenol 1010 (four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester), phosphorous acid ester 168 (three [2.4-di-tert-butyl-phenyl] phosphorous acid ester), vapour bar (Ciba) company of Switzerland; Acid-acceptor ZnO (Hhx121), sea, Zibo is along Xin Ye company limited.
Lubricant: PETS (pentaerythritol stearate), husky (Lonza) company of U.S. dragon.
As shown in Table 1 and Table 2, the proportioning of comparative example 1 ~ 5 and performance are as shown in Table 3 and Table 4 for the proportioning of embodiment 1 ~ 5 and performance.
The composition of table 1 high heat-resistant halogen-free flame-retardant polyphenylene oxide
The performance of table 2 high heat-resistant halogen-free flame-retardant polyphenylene oxide
Remarks: V0, V1 are flame retardant rating, and V0 the highest grade.
The composition of table 3 simultaneous test halogen-free flameproof PPO
The performance of table 4 simultaneous test halogen-free flameproof PPO
Remarks: off grade represents that test bars is burnt to fixture always.
According to the contrast of above-described embodiment 1 with comparative example 1, compared with impact resistant polystyrene (HIPS), adopt the syndiotactic polystyrene (sPS) of high-impact and polyphenylene oxide (PPO) compound, the heat-drawn wire of obtained halogen-free fire-retardant polyphenyl ether significantly improves.This is because syndiotactic polystyrene is the crystalline material of fusing point up to 270 DEG C, and impact resistant polystyrene is then indefinite form material that second-order transition temperature is 90 DEG C.
Known with the contrast of comparative example 2 and comparative example 3 by embodiment 3: (1) phosphate flame retardant PX220 equal proportion replaces red phosphor masterbatch 30450N3, flame retardant resistance obviously declines, become from original V0 rank and do not obtain flame retardant rating, in order to reach V0 rank, need the consumption greatly increasing fire retardant, this is because the available phosphorus content of PX220 only has about 10%, far below the phosphorus content of red phosphor masterbatch 30450N3.(2) adding of phosphate flame retardant PX220 the heat-drawn wire of halogen-free fire-retardant polyphenyl ether is reduced, and along with the increase of its content, heat-drawn wire reduces more, and this is because phosphate flame retardant PX220 has obvious plastification, can lower the heat-drawn wire of material.
Known with the contrast of comparative example 4 by embodiment 2, syndiotactic polystyrene grafted maleic anhydride (sPS-g-MAH) add the shock strength that can significantly improve material, this is because it adds the bonding force that can improve resin and glass, thus improves the ability of material repels external impacts.In addition, the mechanical property being added with raising material of syndiotactic polystyrene grafted maleic anhydride (sPS-g-MAH), makes the heat-drawn wire of material also increase.Known by the contrast of embodiment 4 and comparative example 5, polyphenylene oxide grafted maleic anhydride (PPO-g-MAH) has the effect improving halogen-free fire-retardant polyphenyl ether shock strength and heat-drawn wire equally.
In sum, adopt indefinite form polystyrene with polyphenylene oxide compound with tradition and adopt compared with phosphate flame retardant modification, the present invention carries out halogen-free flameproof modification by the red phosphor masterbatch and glass polyphenylene ether selecting high heat-resisting syndiotactic polystyrene resin, high content of phosphorus, can obtain high heat-resistant halogen-free flame-retardant polyphenylene oxide composite material.In addition, be compatilizer by add PPO or sPS be the grafts of matrix, the impact property of high heat-resistant halogen-free flame-retardant polyphenylene oxide can be improved.High heat-resistant halogen-free flame-retardant polyphenylene oxide composite material of the present invention may be used for flame retardant resistance and the high family's electric car of heat resistant requirements and the field such as electric.
Above-described embodiment is the present invention's preferably embodiment; but embodiments of the present invention are not restricted to the described embodiments; change, the modification done under other any does not deviate from spirit of the present invention and principle, substitute, combine, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (10)
1. a high heat-resistant halogen-free flame-retardant polyphenylene oxide composite material, is characterized in that, this matrix material is made up of following component by weight percentage:
Wherein, the red phosphor masterbatch of described halogen-free flame retardants to be impact resistant polystyrene be carrier.
2. high heat-resistant halogen-free flame-retardant polyphenylene oxide composite material according to claim 1, is characterized in that, the intrinsic viscosity that described polyphenylene oxide measures in 25 DEG C of chloroforms is 0.35 ~ 0.65dL/g.
3. high heat-resistant halogen-free flame-retardant polyphenylene oxide composite material according to claim 1, is characterized in that, described syndiotactic polystyrene is high-impact syndiotactic polystyrene, and its Izod notched impact strength is greater than 10KJ/m
2.
4. high heat-resistant halogen-free flame-retardant polyphenylene oxide composite material according to claim 1, is characterized in that, described glass fibre is alkali-free glass fiber, and filament diameter is 7 ~ 17 μm, chopped length 3 ~ 24mm.
5. high heat-resistant halogen-free flame-retardant polyphenylene oxide composite material according to claim 1, it is characterized in that, described red phosphor masterbatch is be the red phosphor masterbatch that 40% ~ 60%, 500 ~ 1500 object red phosphorus first obtain with impact resistant polystyrene extruding pelletization after stablizer, low-molecular-weight wax are coated again by weight percent.
6. high heat-resistant halogen-free flame-retardant polyphenylene oxide composite material according to claim 1, is characterized in that, described compatilizer is at least one in polyphenylene oxide grafted maleic anhydride or syndiotactic polystyrene grafted maleic anhydride.
7. high heat-resistant halogen-free flame-retardant polyphenylene oxide composite material according to claim 1, is characterized in that, described oxidation inhibitor is the composite antioxidant system of hindered phenol, phosphorous acid ester and acid-acceptor composition.
8. high heat-resistant halogen-free flame-retardant polyphenylene oxide composite material according to claim 1, is characterized in that, described lubricant is pentaerythritol stearate.
9., as a preparation method for the high heat-resistant halogen-free flame-retardant polyphenylene oxide composite material in claim 1 ~ 8 as described in any one, it is characterized in that, the method comprises the following steps:
(1) 30% ~ 50% polyphenylene oxide, 15% ~ 50% syndiotactic polystyrene, 1% ~ 7% halogen-free flame retardants, 2% ~ 6% compatilizer, 0.4% ~ 1.0% oxidation inhibitor and 0.2% ~ 1.0% lubricant are joined mixing machine mixing;
(2) the above-mentioned material mixed is put into the main feeding hopper of twin screw extruder, add the glass fibre of 10% ~ 40% at side feeding hopper, by twin screw extruder extruding pelletization, obtained high heat-resistant halogen-free flame-retardant polyphenylene oxide composite material.
10. the preparation method of high heat-resistant halogen-free flame-retardant polyphenylene oxide composite material according to claim 9, is characterized in that, described mixing time is 3 ~ 5min, and the rotating speed of twin screw extruder is 200 ~ 500r/min, and temperature is 250 ~ 290 DEG C.
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