CN105524461B - A kind of fiber glass reinforced halogen-free flame retardant of resistance to gasoline sPS composites and preparation method thereof - Google Patents
A kind of fiber glass reinforced halogen-free flame retardant of resistance to gasoline sPS composites and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of fiber glass reinforced halogen-free flame retardant of resistance to gasoline sPS composites and preparation method thereof.The sPS composites are formulated by the raw materials by weight of following proportioning：20~40%sPS, 20~40%PA66,10~30% glasses, 6~13% halogen-free flame retardants, 2~8% toughener, 2~8% compatilizers, 0.2~0.8% coupling agent, 0.2~0.6% antioxidant and 0.4~0.8% lubricant.Composite of the present invention has advantages below：PA66 has excellent gasoline-resistant performance and heat resistance, and it is added while can substantially improving sPS petrol-resistances, and sPS heat resistance is influenceed less, to expand its use range；The excellent gasoline-resistant performance having in itself by the microcosmic homogeneity and POE of POE g MAH improvement sPS composites, improves sPS composite gasoline-resistant performances；SPS resins and PA66 resins and the interface cohesion of sPS resins and glass are improved using sPS g MAH, improve sPS composite material interface homogeneity, improves the gasoline-resistant performance of composite.
Description
Technical field
The invention belongs to modified plastics field, and in particular to a kind of fiber glass reinforced halogen-free flame retardant of resistance to gasoline sPS composites
And preparation method thereof.
Background technology
Syndiotactic polytyrene (sPS) is the isostructure polystyrene resin synthesized under metallocene catalyst effect, its
Phenyl ring is arranged alternately in the both sides of macromolecular chain.SPS crystallization rates are fast, also known as highly crystalline polystyrene, have it is excellent it is heat-resisting,
The features such as resistant to chemical etching, resistance to steam, solvent resistance, electric property (dielectric loss is small, proof tracking is high), in many necks
Domain can be with the engineering material such as polybutylene terephthalate (PBT) (PBT), nylon66 fiber (PA66), or even polyphenylene sulfide (PPS), liquid crystal
The special engineered material such as polymer (LCP) are at war with.But sPS oxygen index (OI)s are than relatively low, and petrol-resistance is poor, this gesture
Its application in some fields must be influenceed.
The content of the invention
It is that gasoline can be resistant to by providing one kind to solve the shortcomings that prior art and weak point, primary and foremost purpose of the present invention
There is the fiber glass reinforced halogen-free flame retardant sPS composites of very good mechanical properties and heat resistance simultaneously, can be used for the above
The association areas such as higher electric, mechanical chemical industry can be required.
Another object of the present invention is to provide the preparation side of the above-mentioned fiber glass reinforced halogen-free flame retardant of resistance to gasoline sPS composites
Method.
For achieving the above object, the present invention adopts the following technical scheme that：
A kind of fiber glass reinforced halogen-free flame retardant of resistance to gasoline sPS composites, the composite by syndiotactic polytyrene (sPS),
Nylon66 fiber (PA66), glass (glass fibre), halogen-free flame retardants, toughener, compatilizer, antioxidant and lubricant composition, with weight
Measure percentage to calculate, each component dosage is as follows：
Described compatilizer is sPS-g-MAH (syndiotactic polytyrene grafted maleic anhydride).
SPS is contained in compatilizer sPS-g-MAH one end, and the other end contains what is reacted with PA66 and glass surface polar groups
MAH, it is possible to increase the combination of sPS and PA66 and sPS and glass, play more preferable compatible role.
Preferably, described sPS is high-impact syndiotactic polytyrene, and its Izod notched impact strength is more than 10KJ/m2
(ISO180,23 DEG C).
Preferably, described PA66, its intrinsic viscosity are 2.0~3.4.The molecule of nylon66 fiber of the relative viscosity less than 2.0
Measure too low, material mechanical performance is poor；And relative viscosity is higher than 3.4 nylon66 fiber poor fluidity, processing difficulties are brought.
Preferably, described glass is alkali-free glass fiber, and filament diameter is 7~17 μm, and chopped length is 3~24mm.Directly
Fiber of the footpath less than 7 μm prepares difficulty, and is easily worn during composite processing, and loss of strength is very big；Diameter is big
It can be influenceed and the combination of resin in 17 μm of glasses, the same performance for influenceing composite.In order to increase the knot of glass and resin
With joint efforts, glass surface is handled using silane coupler.
Preferably, the halogen-free flame retardants is red phosphor masterbatch.The red phosphor masterbatch preferably by 50~90 (weight) %,
The red phosphorus of 500~1500 mesh obtains red phosphorus mother with POE-g-MAH extruding pelletizations again after first passing through stabilizer, low-molecular-weight wax cladding
Grain.
Preferably, described toughener is POE-g-MAH (polyethylene glycol oxide grafted maleic anhydride).
Preferably, described coupling agent is that silane coupler is gamma-aminopropyl-triethoxy-silane；
Preferably, described antioxidant is hindered phenol, the compounding antioxidant system of phosphite ester composition；
Preferably, described lubricant is pentaerythritol stearate.
In order to improve sPS oxygen index (OI)s than the shortcomings that relatively low, petrol-resistance is poor, while ensure that material remains in that well
Heat resistance and mechanical performance, it is excellent that the present invention intends adding gasoline-resistant performance, while has superior heat resistance performance and mechanicalness
Can nylon66 fiber (PA66) and sPS it is compound, and add glass and red phosphorus carries out enhancing and flame-retardant modified, prepare the glass of resistance to gasoline and increase
Strong halogen-free flameproof sPS composites.
In order to realize the object of the invention, one aspect of the present invention passes through compatilizer and the preferred solution sPS and PA66 of toughener
The problem of poor compatibility, on the other hand the red phosphor masterbatch of POE-g-MAH carriers is selected to realize the high heat-resistant halogen-free flame-retardant of material.This
Invention uses the sPS with highly polar maleic anhydride (MAH) grafting as compatilizer, while using polyolefin elastomer (POE)
Grafted maleic anhydride carries out toughener to material, improves sPS and PA66 compatibility, material is had excellent mechanicalness
Energy.The red phosphorus halogen-free flame retardants that the present invention uses has highly effective flame-retardant, do not reduce material it is heat-resisting (other halogen-free flame retardants, especially
It is the halogen-free flame retardants of phosphoric acid ester, due to its plasticization, the heat-resisting obvious reduction of material can be made) the characteristics of, while using female
The form of grain, it can be improved while red phosphorus stability is ensured and disperseed, so as to improve processing characteristics and fire resistance.
A kind of preparation method for preparing the above-mentioned fiber glass reinforced halogen-free flame retardant of resistance to gasoline sPS composites, comprises the following steps：
Coupling agent and halogen-free flame retardants are first mixed into 3~5min in 80~100 DEG C, then add sPS, PA66, toughener agent, compatible
Agent, antioxidant and lubricant mix 3~5min in 60~80 DEG C, and mixed material finally is added into extruder main feeding hopper,
In side, feeding hopper adds 10~30% glass, and by double screw extruder extruding pelletization, the fiber glass reinforced halogen-free of resistance to gasoline is made
Fire-retardant sPS composites.The rotating speed of double screw extruder is 300~500r/min, and temperature is 260~300 DEG C.
Compared with prior art, the present invention has advantages below and beneficial effect：
(1) PA66 has excellent gasoline-resistant performance and heat resistance, and its addition can substantially improve sPS petrol-resistances
Meanwhile sPS heat resistance is influenceed less, to expand its use range.
(2) using sPS-g-MAH as compatilizer, it is possible to increase sPS resins and PA66 resins and sPS resins and glass
Interface cohesion, improve sPS composite material interface homogeneity, improve the gasoline-resistant performance of composite.
(3) using red phosphor masterbatch, its high content of phosphorus can reduce the addition of fire retardant for halogen-free flame retardants；Red phosphorus is inorganic
The characteristic of filler will not reduce the heat resistance of material；Processing characteristics and fire resistance can be improved using master batch form.
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,
Described embodiment is only part of the embodiment of the present invention, rather than whole embodiments.Based on the implementation in the present invention
Example, all other embodiment that those of ordinary skill in the art are obtained under the premise of creative work is not made, is belonged to
The scope of protection of the invention.
The embodiment of the present invention and comparative example are molded into the standard batten of test according to standard requirement and tested.Its
In, tensile strength according to ISO527 standards, vertical combustion according to UL94 standards (1.6mm), heat distortion temperature test according to
ISO75-2 standards (0.45MPa).Gasoline-resistant performance soaks the holding of 100 hours post-tensioning intensity using batten in No. 95 gasoline
Rate is assessed, and specific test process is as follows：(1) tensile bars are positioned in the closed glass jar equipped with No. 95 gasoline, sample
Bar is completely soaked in the oil；(2) vial equipped with batten is positioned in 80 DEG C of constant temperature oven；Will after (3) 100 hours
Batten takes out, and is positioned over 23 DEG C after taking out surface oil stain, carries out extension test after 24 hours in the incubator of humidity 50%, each
5 battens of condition test and using average value as test result, and tensile strength calculated is relative to the percentage of initial tensile strength.
The raw material used in the embodiment of the present invention and comparative example is as follows：
sPS：XARECTMS105 (Izod notched impact strength 20KJ/m2, ISO180,23 DEG C), Japanese light extraction
(Idemitsu) company；
PA66：PA66EPR27 (intrinsic viscosity 2.7), China Shenma Group Co., Ltd.；
Glass ECS3014B：13 μm, chopped length 4.5mm of filament diameter, Chongqing Polycomp International Co., Ltd；
Halogen-free flame retardants：FRP-950X (red phosphor masterbatch, microcapsule red phosphorus content 80%, POE-g-MAH carriers) Guangzhou
Yin Su fire proofings Co., Ltd；
Toughener：FUSN493D (POE-g-MAH), Dupont (DuPont) company；FG1901 (SEBS-g-MAH) is beautiful
(Kraton) company is risen by section of state；
Compatilizer：9012PA (sPS-g-MAH), German Bi Ke (BYK) company；
Coupling agent：KBM-903 (gamma-aminopropyl-triethoxy-silane), Japanese SHIN-ETSU HANTOTAI (Shinetsu) company；
Antioxidant：Hindered phenol 1098 (N, N'- pairs-(3- (3,5- di-tert-butyl-hydroxy phenyl) propiono) hexamethylene diamine),
Phosphite ester S-9228 (double (2,4-two cruel bases) pentaerythritol diphosphites), the U.S. all good fortune (Dover) company；
Lubricant：PETS (pentaerythritol stearate), husky (Lonza) company of U.S. dragon.
Embodiment 1
A kind of preparation method of the fiber glass reinforced halogen-free flame retardant of resistance to gasoline sPS composites, comprises the following steps：
(1) sPS, PA66, halogen-free flame retardants, toughener, compatilizer, glass, coupling agent, antioxidant and lubrication in table 1 are pressed
The amount of agent weighs raw material；
(2) coupling agent and halogen-free flame retardants are mixed into 5min in 80 DEG C, then adds sPS, PA66, toughener, compatible
Agent, antioxidant and lubricant mix 5min in 60 DEG C, then add extruder main feeding hopper, and in side, feeding hopper adds glass, leads to
Cross double screw extruder extruding pelletization.
The rotating speed of double screw extruder is 400r/min, and temperature is 260~300 DEG C.The fiberglass reinforced of resistance to gasoline of gained without
The fire-retardant sPS composite properties of halogen are shown in Table 2.
Embodiment 2
A kind of preparation method of the fiber glass reinforced halogen-free flame retardant of resistance to gasoline sPS composites, comprises the following steps：(1) table 1 is pressed
Middle sPS, PA66, halogen-free flame retardants, toughener, compatilizer, glass, coupling agent, the amount of antioxidant and lubricant weigh raw material；
(2) coupling agent and halogen-free flame retardants are mixed into 3min in 100 DEG C, then adds sPS, PA66, toughener, compatible
Agent, antioxidant and lubricant mix 3min in 80 DEG C, then add extruder main feeding hopper, and in side, feeding hopper adds glass, leads to
Cross double screw extruder extruding pelletization.
The rotating speed of double screw extruder is 500r/min, and temperature is 260~300 DEG C.The fiberglass reinforced of resistance to gasoline of gained without
The fire-retardant sPS composite properties of halogen are shown in Table 2.
Embodiment 3
A kind of preparation method of the fiber glass reinforced halogen-free flame retardant of resistance to gasoline sPS composites, comprises the following steps：
(1) sPS, PA66, halogen-free flame retardants, toughener, compatilizer, glass, coupling agent, antioxidant and lubrication in table 1 are pressed
The amount of agent weighs raw material；
(2) coupling agent and halogen-free flame retardants are mixed into 3min in 90 DEG C, then adds sPS, PA66, toughener, compatible
Agent, antioxidant and lubricant mix 4min in 70 DEG C, then add extruder main feeding hopper, and in side, feeding hopper adds glass, leads to
Cross double screw extruder extruding pelletization.
The rotating speed of double screw extruder is 350r/min, and temperature is 260~300 DEG C.The fiberglass reinforced of resistance to gasoline of gained without
The fire-retardant sPS composite properties of halogen are shown in Table 2.
Embodiment 4~5
After embodiment 4~5 weighs raw material by table 1 respectively, the fiberglass reinforced of resistance to gasoline is prepared according to the method for embodiment 1
Halogen-free flameproof sPS composites, the fiber glass reinforced halogen-free flame retardant of the resistance to gasoline sPS composite properties of gained are shown in Table 2.
Comparative example 1~5
After comparative example 1~5 weighs raw material according to table 3 respectively, modification is prepared by used sPS conventional method
SPS samples.The modification sPS properties of sample detection of gained is shown in Table 4.
The composition of the fiber glass reinforced halogen-free flame retardant of the resistance to gasoline sPS composites of table 1
The embodiment performance detection of table 2
| Heat distortion temperature/DEG C | Combustibility | Gasoline-resistant performance/% | |
| Embodiment 1 | 244 | V0 | 78.2 |
| Embodiment 2 | 251 | V0 | 80.3 |
| Embodiment 3 | 253 | V2 | 76.4 |
| Embodiment 4 | 256 | V0 | 55.3 |
| Embodiment 5 | 250 | V0 | 49.3 |
The composition of the comparative example sPS composites of table 3
The comparative example performance detection of table 4
| Heat distortion temperature/DEG C | Combustibility | Gasoline-resistant performance/% | |
| Comparative example 1 | 240 | V2 | 21.2 |
| Comparative example 2 | 260 | V0 | 70.3 |
| Comparative example 3 | 238 | V0 | 42.6 |
| Comparative example 4 | 252 | Off grade | 68.3 |
| Comparative example 5 | 228 | Off grade | 54.5 |
PA66 addition is can be seen that by the comparison to comparative example 1 and embodiment 1 can be obviously improved sPS composite woods
The gasoline-resistant performance of material, this is due to that PA66 has excellent gasoline-resistant performance.
Toughener FUSN493D addition is can be seen that by the comparison of comparative example 2 and embodiment 2 can improve sPS and answer
The gasoline-resistant performance of condensation material.This is due to that FUSN493D is POE-g-MAH, itself has excellent gasoline-resistant performance, together
When can improve the interface cohesion of resin and glass, lower erosion of the gasoline to sPS.
By the contrast of comparative example 3 and embodiment 4 can be seen that addition compatilizer 9012PA can improve improve sPS answer
The gasoline-resistant performance of condensation material.This is due to the compatibility that 9012PA can improve sPS and PA66 and glass, enhancing interface knot
With joint efforts, so as to reducing infringement of the gasoline to sPS resins.Further, since the enhancing of interface binding power, the thermal deformation of embodiment 4
Heat distortion temperature of the temperature apparently higher than comparative example 3.
By the contrast of comparative example 4 and embodiment 3 as can be seen that the addition of red phosphor masterbatch can improve sPS composites
Fire resistance.It is can be seen that by the contrast of comparative example 5 and embodiment 5 under identical addition, the fire-retardant effect of red phosphor masterbatch
Fruit is substantially better than OP1312 fire resistance, and this is due to that red phosphor masterbatch phosphorus content is higher, has higher flame retarding efficiency.Together
When, the heat distortion temperature of embodiment 5 apparently higher than comparative example 5 heat distortion temperature, this be due to OP1312 for phosphoric acid ester without
Halogen fire retardant, there is obvious plasticization, the heat distortion temperature of material can be reduced, and red phosphorus is inorganic filler, its addition pair
Heat distortion temperature influences smaller.
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)
- A kind of 1. fiber glass reinforced halogen-free flame retardant of resistance to gasoline sPS composites, it is characterised in that the composite by sPS, PA66, Glass, halogen-free flame retardants, toughener, compatilizer, antioxidant and lubricant composition, calculated in weight percent, each component dosage It is as follows：Described compatilizer is sPS-g-MAH；Described toughener is POE-g-MAH；Described glass is alkali-free glass fiber, and single A diameter of 7~17 μm of silk, 3~24mm of chopped length.
- A kind of 2. fiber glass reinforced halogen-free flame retardant of resistance to gasoline sPS composites according to claim 1, it is characterised in that institute The sPS stated is high-impact syndiotactic polytyrene, and its Izod notched impact strength is more than 10KJ/m2。
- A kind of 3. fiber glass reinforced halogen-free flame retardant of resistance to gasoline sPS composites according to claim 1, it is characterised in that institute The PA66 stated, its intrinsic viscosity are 2.0~3.4.
- A kind of 4. fiber glass reinforced halogen-free flame retardant of resistance to gasoline sPS composites according to claim 1, it is characterised in that institute The halogen-free flame retardants stated is red phosphor masterbatch.
- A kind of 5. fiber glass reinforced halogen-free flame retardant of resistance to gasoline sPS composites according to claim 1, it is characterised in that institute The coupling agent stated is that silane coupler is gamma-aminopropyl-triethoxy-silane；Described antioxidant is hindered phenol and phosphite ester The compounding antioxidant system of composition.
- A kind of 6. fiber glass reinforced halogen-free flame retardant of resistance to gasoline sPS composites according to claim 1, it is characterised in that institute The lubricant stated is pentaerythritol stearate.
- A kind of 7. preparation side of the fiber glass reinforced halogen-free flame retardant of resistance to gasoline sPS composites described in any one of claim 1 to 6 Method, it is characterised in that comprise the following steps：(1) by weight percentage, 0.2~0.8% coupling agent and 6~13% halogen-free flame retardants are first mixed 3 in 80~100 DEG C ~5min, then add 20~40%sPS, 20~40%PA66,2~8% toughener, 2~8% compatilizers, 0.2~ 0.6% antioxidant and 0.4~0.8% lubricant mix 3~5min in 60~80 DEG C；(2) the above-mentioned material mixed is added into extruder main feeding hopper, and 10~30% glasses is added in the feeding hopper of side, so Afterwards by double screw extruder extruding pelletization, the fiber glass reinforced halogen-free flame retardant of resistance to gasoline sPS composites, double screw extruder is made Rotating speed be 200~500r/min, temperature is 260~300 DEG C.
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| CN105754243A (en) * | 2016-05-12 | 2016-07-13 | 广州市聚赛龙工程塑料股份有限公司 | Conductive high-heat-resistant halogen-free flame retardant sPS composite and preparation method thereof |
| CN106751075A (en) * | 2016-11-28 | 2017-05-31 | 古道尔工程塑胶（深圳）有限公司 | Syndiotactic polytyrene polyhexamethylene adipamide flame-proof composite material |
| CN106751077B (en) * | 2016-11-28 | 2019-11-29 | 古道尔工程塑胶（深圳）有限公司 | Syndiotactic polytyrene flame retardant composite material |
| CN108485098A (en) * | 2018-04-18 | 2018-09-04 | 广州找塑料新材料科技有限公司 | Vinal enhances the high creepage trace syndiotactic polytyrene composite material of halogen-free flameproof and preparation method |
| CN110951177A (en) * | 2019-12-13 | 2020-04-03 | Oppo广东移动通信有限公司 | Nano-injection composite material and preparation method thereof, housing assembly and electronic device |
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| US5270353A (en) * | 1989-02-10 | 1993-12-14 | Idemitsu Kosan Co., Ltd. | Resin composition |
| JP2001516786A (en) * | 1997-09-12 | 2001-10-02 | ザ ダウ ケミカル カンパニー | Toughened polymer blend |
| CN1164670C (en) * | 2001-04-04 | 2004-09-01 | 中国石油化工股份有限公司 | Syndiotactic polyphenylethylene/polyamide composite material |
| CN104693629A (en) * | 2013-12-06 | 2015-06-10 | 上海杰事杰新材料(集团)股份有限公司 | A flame-retardant polystyrene/polyamide blended alloy material and a preparing method thereof |
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