CN106280462A - A kind of high-impact height CTI polyphenyl thioether composite material and its preparation method and application - Google Patents
A kind of high-impact height CTI polyphenyl thioether composite material and its preparation method and application Download PDFInfo
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- CN106280462A CN106280462A CN201610824544.9A CN201610824544A CN106280462A CN 106280462 A CN106280462 A CN 106280462A CN 201610824544 A CN201610824544 A CN 201610824544A CN 106280462 A CN106280462 A CN 106280462A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L81/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing sulfur with or without nitrogen, oxygen or carbon only; Compositions of polysulfones; Compositions of derivatives of such polymers
- C08L81/02—Polythioethers; Polythioether-ethers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
- C08L77/06—Polyamides derived from polyamines and polycarboxylic acids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/004—Additives being defined by their length
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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Abstract
The invention belongs to modified plastics field, specifically disclose a kind of high-impact height CTI polyphenyl thioether composite material and its preparation method and application.Described composite is made up of polyphenylene sulfide, nylon66 fiber, toughener, glass, antioxidant, lubricant and coupling agent.The present invention is directed to the shortcoming that PPS resin is susceptible to tracking failure, add the PA66 resin with high CTI, PA66 adds in addition to improving the CTI of PPS composite, its impact strength can also be improved, and by the further toughening effect of the efficient toughener of PA66, it is thus achieved that there is the PPS composite of high-impact performance height CTI.The present invention is simple to operate, it is thus achieved that high-impact height CTI PPS composite cost relatively low, there is good marketing prospect.Described composite has superior shock resistance energy, excellent anti-electric-mark destructive characteristics, may be used for the association area such as electric higher to above performance requirement.
Description
Technical field
The invention belongs to modified plastics field, be specifically related to a kind of high-impact height CTI polyphenyl thioether composite material and system thereof
Preparation Method and application.
Background technology
As the first big special engineering plastics, polyphenylene sulfide (PPS) has the combination property of excellence, is embodied in prominent
Heat stability, fire resistance, excellent chemical resistance, creep resistant, electrical insulating property and processing forming.PPS is due to excellent
Performance, have a wide range of applications in electric field, but its some existed is not enough to be affected it and further apply.
PPS molecular backbone is alternately arranged by phenyl ring and sulphur atom, and chain regularity is very strong, so it is easy to crystallization, this is
While it brings high heat-resisting and high rigidity, also make it that shortcoming that impact strength is low occurs.The deficiency of toughness makes answering of PPS
With being subject to certain restrictions, although the addition of the reinforcing materials such as glass, carbon are fine can improve its toughness to a certain extent, but this is full
The high-impact requirement that material is proposed by foot the most electric integrated, lightweight and the development that becomes more meticulous.
On the other hand, although PPS has good electrical insulation capability, but, owing to it becomes carbon performance, good feature causes
It is susceptible to tracking failure.Tracking failure produces carbide at material surface, forms tungsten carbide/conductive road, and stretches to electrode direction
Exhibition, can cause short circuit time serious, damage electric component, therefore improve the relative discharge tracking index (Comparative of PPS
Tracking Index), i.e. CTI, could expand its application in electric field further.
Chinese patent CN 1314762C discloses a kind of high toughness packing reinforced polyphenyl thioether composite material and preparation side thereof
Method.Its composition includes: PPS25～65%, glass fibre 20～50%, inorganic mineral 0～40%, impact modifying agent 3～10%,
Coupling agent 0.2～1%, antioxidant 0.2～0.5%, processing aid 0.5～2%.The impact modifying agent that this patent uses is hydrogenation
SBS or styrene butyl acrylate binary graft modification EP rubbers (EPDM-g-St) and ethylene-methyl methacrylate (+)-2,3-Epoxy-1-propanol
The blend of ester.Although the addition of toughener can improve the impact strength strengthening PPS, but improvement amplitude is not very big, meanwhile,
The existence of inorganic filler also can affect the toughening effect of toughener.
Chinese patent CN 102276982B discloses a kind of polyphenylene sulfide and high-temperature-resistant nylon complex and preparation side thereof
Method.High temperature resistant nylon used is one or more mixture in PA46, PA6T, PA9T, and compatilizer used is maleic acid
The mixing of one or more in acid anhydride Maleated SEBS, maleic anhydride graft phenylethene, maleic anhydride grafted ethene octene copolymer
Thing.Although the addition of high-temperature nylon and compatilizer can improve the impact strength of fiberglass reinforced PPS, but owing to high-temperature nylon supplies
Answer the feature that channel is single and with high costs, be unfavorable for large-scale production and popularization.Chinese patent CN 104277459 A class
As also disclose a kind of polyphenylene sulfide/semi-aromatic nylon composite and preparation method thereof, but it is high to equally exist cost, no
The shortcoming that profit is promoted.
Above patent is mainly for the toughening modifying of PPS, and the CTI to PPS does not does relevant assessment.Chinese patent CN
102924921 A disclose a kind of high phase ratio creepage tracking index polyphenylene sulfide and strengthen composite and preparation technology thereof.Its group
One-tenth includes: PPS25～40%, glass 25～40%, filler 25～40%, coupling agent 0.3～1%, antioxidant 0.3～1%,
Lubricant 0.1～1%.Compounded by chopped glass fiber and ultra-fine filling mineral so that the CTI of PPS composite reach 225V with
On, but due to the addition of a large amount of mineral and do not have effective toughened system, the impact strength causing PPS composite is the highest.
Chinese patent CN 104194337 A uses polyethylene to connect with ethylene-methyl methacrylate (+)-2,3-Epoxy-1-propanol fat or polyolefin elastomer
The (+)-2,3-Epoxy-1-propanol ester blend of branch improves impact property and the CTI of PPS as impact modifying agent, but its improvement amplitude failing to understand
Aobvious, particularly CTI is the highest less than 200V.
Summary of the invention
In place of shortcoming and defect for solution prior art, the primary and foremost purpose of the present invention is to provide a kind of high-impact high
CTI polyphenyl thioether composite material.This composite has superior shock resistance energy, excellent anti-electric-mark destructive characteristics, may be used for
The association area such as electric higher to above performance requirement.
Another object of the present invention is to provide the preparation method of above-mentioned high-impact height CTI polyphenyl thioether composite material.
The object of the invention is achieved through the following technical solutions:
A kind of high-impact height CTI polyphenyl thioether composite material, this composite is by polyphenylene sulfide (PPS), nylon66 fiber
(PA66), glass, toughener, antioxidant, lubricant and coupling agent composition, calculated in weight percent, each amounts of components is as follows:
Preferably, described PPS melt flow rate is 200～800g/min (test condition 316 DEG C, 5kg).Melt-flow
When dynamic speed is less than 200g/min, PPS mobility is poor, is unfavorable for processing, and when molten flow rate is more than 800g/min, PPS
Molecular weight is the least, and the PPS composite machinery performance prepared and thermostability are poor.
Preferably, described PPS weight average molecular weight is 20000～60000.
Preferably, described PA66, relative viscosity is 2.0～3.4.Relative viscosity is less than the molecular weight mistake of 2.0 nylon66 fiber
Low, material mechanical performance is poor, and relative viscosity is higher than 3.4 nylon66 fiber poor fluidities, brings processing difficulties.
Preferably, described glass (i.e. glass fibre) is alkali-free glass fiber (i.e. alkali-free glass fibre), and filament diameter is 7
～17 μm, chopped length 3～24mm.Diameter is difficult less than the fiber preparation of 7 μm, and during composite processing easily
Abrasion, loss of strength is the biggest；Diameter can affect the combination with resin more than the glass of 17 μm, affects the property of composite equally
Energy.In order to increase the adhesion of glass and resin, glass surface uses silane coupler to process.
Preferably, described toughener is POE-g-MAH (polyethylene glycol oxide grafted maleic anhydride).
Preferably, described coupling agent is silane coupler；More preferably gamma-aminopropyl-triethoxy-silane.
Preferably, described antioxidant is hindered phenol and the compounding antioxidant system of phosphite ester composition.
Preferably, described lubricant is silicone powder.
Add with PPS solubility parameter close to (compatible than relatively low shortcoming, the present invention to improve PPS composite CTI
Property is good), there is the PA66 resin of excellent CTI performance simultaneously.The addition of PA66 resin, except improving the CTI of PPS composite
Outward, it is also possible to significantly improve its impact strength.On the other hand, owing to PPS Polarity comparision is weak, general toughener does not has very well
Toughening effect, by introducing PA66, the efficient toughener of PA66 can be used, by its toughening effect to PA66, improve PPS
The toughness of composite.
The present invention easily carries out toughening modifying and has the PA66 of excellent CTI performance by introducing simultaneously and carry out PPS material
Modification, and toughness reinforcing by fiberglass reinforced and toughener, obtain the PPS composite with high-impact height CTI.
A kind of preparation method preparing above-mentioned high-impact height CTI polyphenyl thioether composite material, comprise the steps: by PPS,
Coupling agent, after 120～140 DEG C of mixing 8～10min, is cooled to 60～80 DEG C, adds PA66, coupling agent, toughener, antioxygen
Agent, mix lubricant 3～5min, add extruder main feeding hopper by mixed material, adds 30～50% at side feeding hopper
Glass, by double screw extruder extruding pelletization, prepare high-impact height CTI polyphenyl thioether composite material.
The present invention uses the method that PPS resin powder particle and coupling agent are the most at high temperature blended, and this is due at height
Under temperature, coupling agent viscosity is relatively low, and PPS resin powder particle occurs certain expansion to produce more micropores, beneficially coupling agent simultaneously
Preferably it is coated with PPS resin.
The rotating speed of described double screw extruder is 300～500r/min, and temperature is 260～300 DEG C.
Compared with prior art, the present invention has the following advantages and beneficial effect:
(1) add PA66, the CTI of PPS composite can be significantly improved, expand PPS composite at electric neck
The application in territory；
(2) it is used alone PA66 and i.e. can be obviously improved the impact strength of fiberglass reinforced PPS composite, add PA66 high
Effect toughener, can improve impact strength, it is thus achieved that the PPS composite of high-impact further；
(3) regulating and controlling with by PPS molecular chain structure or compared with adding high-temperature nylon, the present invention uses and is easily obtained
PA66 improves impact strength and the CTI of PPS, and the PPS composite of the present invention is easier to realize industrialization and produces, cost simultaneously
Lower, beneficially marketing.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited to this.
The embodiment of the present invention and comparative example are all molded into the standard batten of test according to standard-required and test.Draw
Stretch test according to ISO527 standard, crooked test according to ISO178 standard, Izod notched impact strength according to ISO180 standard,
CTI tests according to IEC60112 standard.
The raw material used in the embodiment of the present invention and comparative example is as follows:
PPS:PPS1350C, melt flow rate is 450g/min (test condition 316 DEG C, 5Kg), and Zhejiang is new and becomes special type
Materials Co., Ltd；
PA66:PA66EPR27 (relative viscosity 2.7), China Shenma Group Co., Ltd.；
Glass ECS3014B: alkali-free glass fiber, filament diameter 13 μm, chopped length 4.5mm, the world, Chongqing composite is limited
Company；
Glass T635B: alkali-free glass fiber, filament diameter 13 μm, Taishan glass fiber Ltd；
Toughener: FUSN493D (POE-g-MAH), Dupont (DuPont) company；
Coupling agent: KBM-903 (gamma-aminopropyl-triethoxy-silane), SHIN-ETSU HANTOTAI (Shinetsu) company of Japan；
Antioxidant: hindered phenol 1098 (N, N'-pair-(3-(3,5-di-tert-butyl-hydroxy phenyl) propiono) hexamethylene diamine),
BASF (Basf) company of Germany；Phosphite ester S-9228 (double (2,4 two cruel base) pentaerythritol diphosphites), the U.S. is all
Good fortune (Dover) company；
Lubricant: TEGOMER E525 (silicone powder), wins wound (Evonik) industrial group.
Embodiment 1
The preparation method of a kind of high-impact height CTIPPS composite, comprises the following steps:
(1) raw material is weighed by the amount of PPS, PA66, toughener, coupling agent, antioxidant and lubricant in table 1；
(2) by PPS, coupling agent after 120 DEG C of mixing 10min, it is cooled to 60 DEG C, adds PA66, toughener, antioxidant
With mix lubricant 5min, it is subsequently adding extruder main feeding hopper, adds glass at side feeding hopper, squeezed by double screw extruder
Go out pelletize.
The rotating speed of double screw extruder is 400r/min, and temperature is 260～300 DEG C.The high-impact height CTIPPS of gained is multiple
Condensation material performance is shown in Table 2.
Embodiment 2
The preparation method of a kind of high-impact height CTIPPS composite, comprises the following steps:
(1) raw material is weighed by the amount of PPS, PA66, toughener, coupling agent, antioxidant and lubricant in table 1；
(2) by PPS, coupling agent after 130 DEG C of mixing 9min, it is cooled to 70 DEG C, adds PA66, toughener, antioxidant
With mix lubricant 4min, it is subsequently adding extruder main feeding hopper, adds glass at side feeding hopper, squeezed by double screw extruder
Go out pelletize.
The rotating speed of double screw extruder is 300r/min, and temperature is 260～300 DEG C.The high-impact height CTIPPS of gained is multiple
Condensation material performance is shown in Table 2.
Embodiment 3
The preparation method of a kind of high-impact height CTIPPS composite, comprises the following steps:
(1) raw material is weighed by the amount of PPS, PA66, toughener, coupling agent, antioxidant and lubricant in table 1；
2) by PPS, coupling agent 140 DEG C mixing 8min after, be cooled to 80 DEG C, add PA66, toughener, antioxidant and
Mix lubricant 3min, is subsequently adding extruder main feeding hopper, adds glass at side feeding hopper, is extruded by double screw extruder
Pelletize.
The rotating speed of double screw extruder is 500r/min, and temperature is 260～300 DEG C.The high-impact height CTIPPS of gained is multiple
Condensation material performance is shown in Table 2.
Embodiment 4～5
After embodiment 4～5 weighs raw material by table 1 respectively, prepare high-impact height CTIPPS according to the method for embodiment 1
Composite, the high-impact height CTIPPS composite property of gained is shown in Table 2.
Comparative example 1～5
After comparative example 1～5 weighs raw material according to table 3 respectively, prepare modification by the conventional method of existing PPS
PPS sample.The MODIFIED PP S properties of sample detection of gained is shown in Table 4.
The composition of table 1 high-impact height CTIPPS composite
Table 2 embodiment performance detects
The composition of table 3 comparative example PPS composite
Table 4 comparative example performance detects
By comparative example 1 it can be seen that the PPS composite CTI of simple fiberglass reinforced is the lowest, only 125V, rushes simultaneously
Hit intensity is the highest.
PPS composite can be significantly improved it can be seen that add PA66 by the comparison of comparative example 2 with embodiment 2
Impact strength is (by 10.4KJ/m2Become 18.5KJ/m2) and CTI (being become 300V from 150V).
By the comparison of comparative example 3 and embodiment 3 it can be seen that use chopped glass fiber ESC3014B to compare continuous glass-fiber
The mechanical performance that T635B obtains material is higher, and this is owing to chopped glass fiber dispersibility is more preferable, simultaneously as the special glass of nylon,
Its surface conditioning agent is more preferable with the PA66 compatibility, is conducive to improving resin and the bond strength of glass.
By the comparison of comparative example 4 and embodiment 4 it can be seen that the addition of toughener (FUSN493D) can carry further
The impact strength of high PPS composite, this is owing to it is the efficient toughener of PA66, compound by bringing PA66 toughness reinforcing
The rising of material impact intensity.And FUSN493D does not substantially have toughening effect to pure PPS, this be due on PPS strand also
Not having the polar functional group that can react with FUSN493D, this can also be verified from comparative example 2, although contains in system
The FUSN493D of up to 8%, but the impact strength of PPS composite is the highest.
By the contrast of comparative example 5 and embodiment 2 it can be seen that when FUSN493D addition is 9%, PPS composite wood
The impact property of material does not only have further up, presents downward trend on the contrary, and this is due to along with the increasing of FUSN493D content
Adding, it combines contribution decline to improving between resin and glass, simultaneously because it affects material flowability, affect resin to glass
Infiltration and cladding, decohesion degree between resin and glass is risen by it, under this disappears and other rises, causes impact property to decline.
Above-described embodiment is the present invention preferably embodiment, but embodiments of the present invention are not by above-described embodiment
Limit, the change made under other any spirit without departing from the present invention and principle, modify, substitute, combine, simplify,
All should be the substitute mode of equivalence, within being included in protection scope of the present invention.
Claims (9)
1. a high-impact height CTI polyphenyl thioether composite material, it is characterised in that described composite by polyphenylene sulfide, PA66,
Glass, toughener, antioxidant, lubricant and coupling agent composition, calculated in weight percent, each amounts of components is as follows:
。
A kind of high-impact height CTI polyphenyl thioether composite material the most according to claim 1, it is characterised in that described is poly-
Diphenyl sulfide melt flow rate is 200～800g/min.
A kind of high-impact height CTI polyphenyl thioether composite material the most according to claim 1, it is characterised in that described
PA66, relative viscosity is 2.0～3.4.
A kind of high-impact height CTI polyphenyl thioether composite material the most according to claim 1, it is characterised in that described glass
Fibre is alkali-free glass fiber, and filament diameter is 7～17 μm, chopped length 3～24mm.
A kind of high-impact height CTI polyphenyl thioether composite material the most according to claim 1, it is characterised in that described increasing
Tough dose is POE-g-MAH.
A kind of high-impact height CTI polyphenyl thioether composite material the most according to claim 1, it is characterised in that described idol
Connection agent is silane coupler；Described antioxidant is hindered phenol and the compounding antioxidant system of phosphite ester composition；Described lubrication
Agent is silicone powder.
7. the preparation method of the high-impact height CTI polyphenyl thioether composite material described in any one of claim 1 to 6, its feature exists
In, comprise the steps: by weight percentage, by 20～40% polyphenylene sulfide, 0.6～1.0% coupling agent and 120～140
After DEG C mixing 8～10min, it is cooled to 60～80 DEG C, adds 10～30%PA66,2～8% toughener, 0.2～0.6% anti-
Oxygen agent, 0.2～0.8% mix lubricant 3～5min, add extruder main feeding hopper by mixed material, at side feeding hopper
Addition 30～the glass of 50%, by double screw extruder extruding pelletization, prepare high-impact height CTI polyphenyl thioether composite material.
The preparation method of high-impact height CTI polyphenyl thioether composite material the most according to claim 7, it is characterised in that institute
The rotating speed stating double screw extruder is 300～500r/min, and temperature is 260～300 DEG C.
9. the answering in electric field of the high-impact height CTI polyphenyl thioether composite material described in any one of claim 1 to 6
With.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107189437A (en) * | 2017-06-26 | 2017-09-22 | 苏州市慧通塑胶有限公司 | PPS PA66 short glass fiber high molecule alloy materials and preparation method thereof |
| CN110204899A (en) * | 2019-06-10 | 2019-09-06 | 大河宝利材料科技(苏州)有限公司 | The preparation method of fiberglass enhanced polyphenyl thioether composite material |
| CN110791095A (en) * | 2018-08-01 | 2020-02-14 | 山东赛恩吉新材料有限公司 | Polyphenylene sulfide composite material and preparation method and application thereof |
| WO2022110668A1 (en) * | 2020-11-30 | 2022-06-02 | 金发科技股份有限公司 | Highly hydrophobic cti polyphenylene sulfide composition, preparation method therefor and application thereof |
| CN117186643A (en) * | 2023-09-20 | 2023-12-08 | 浙江兄弟新材料有限公司 | Polyphenylene sulfide composite material with ultrahigh relative electric leakage tracking index and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107189437A (en) * | 2017-06-26 | 2017-09-22 | 苏州市慧通塑胶有限公司 | PPS PA66 short glass fiber high molecule alloy materials and preparation method thereof |
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| CN110791095B (en) * | 2018-08-01 | 2021-08-10 | 山东赛恩吉新材料有限公司 | Polyphenylene sulfide composite material and preparation method and application thereof |
| CN110204899A (en) * | 2019-06-10 | 2019-09-06 | 大河宝利材料科技(苏州)有限公司 | The preparation method of fiberglass enhanced polyphenyl thioether composite material |
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| CN117186643A (en) * | 2023-09-20 | 2023-12-08 | 浙江兄弟新材料有限公司 | Polyphenylene sulfide composite material with ultrahigh relative electric leakage tracking index and preparation method thereof |
| CN117186643B (en) * | 2023-09-20 | 2024-06-18 | 浙江兄弟新材料有限公司 | Polyphenylene sulfide composite material with ultrahigh relative electric leakage tracking index and preparation method thereof |
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Application publication date: 20170104 |