CN106987120A - A kind of oil resistant high CTI value halogen free flame-retardant polyphenylene oxide composite material and preparation method thereof - Google Patents
A kind of oil resistant high CTI value halogen free flame-retardant polyphenylene oxide composite material and preparation method thereof Download PDFInfo
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- CN106987120A CN106987120A CN201710260437.2A CN201710260437A CN106987120A CN 106987120 A CN106987120 A CN 106987120A CN 201710260437 A CN201710260437 A CN 201710260437A CN 106987120 A CN106987120 A CN 106987120A
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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
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L71/00—Compositions of polyethers obtained by reactions forming an ether link in the main chain; Compositions of derivatives of such polymers
- C08L71/08—Polyethers derived from hydroxy compounds or from their metallic derivatives
- C08L71/10—Polyethers derived from hydroxy compounds or from their metallic derivatives from phenols
- C08L71/12—Polyphenylene oxides
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- 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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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K2201/004—Additives being defined by their length
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- C—CHEMISTRY; METALLURGY
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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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
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/22—Halogen free composition
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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
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
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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, a kind of oil resistant high CTI value halogen free flame-retardant polyphenylene oxide composite material and preparation method thereof is specifically disclosed.The composite is made up of polyphenylene oxide, nylon66 fiber, halogen-free flame retardants, compatilizer, toughener, glass, antioxidant and lubricant.The shortcoming of tracking failure and oil resistivity difference easily occurs for PPE resins for the present invention, adds tool PA66 resins and glass, and uses red phosphor masterbatch for halogen-free flame retardants, and PA66 addition can be obviously improved the CTI and oil resistance of PPE composites；The addition of glass can improve the heat resistance and oil resistance of composite；The characteristics of red phosphor masterbatch has highly effective flame-retardant, can improve the fire resistance of PPE composites, while will not be decreased obviously the heat resistance and CTI values of material.The present invention is simple to operate, and the oil resistant high CTI value halogen free flame-retardant polyphenylene oxide composite material cost of acquisition is relatively low, with good market promotion prospect.
Description
Technical field
The invention belongs to modified plastics field, and in particular to a kind of oil resistant high CTI value halogen free flame-retardant polyphenylene oxide composite material
And preparation method thereof.
Background technology
Polyphenylene oxide (PPE) is small with relative density as one of five large-engineering materials, and proof stress is loose, creep resistance, resistance to
A series of excellent properties such as heat, resistant to hydrolysis, resistance to vapor, dimensional stability, while having fire retardant self-extinguishment and in very wide temperature
The features such as excellent electric performance being kept in degree, frequency range.PPE has extensive due to excellent performance in electric field
Application, but its some not enough influence for existing its further apply.
Although PPE is with good electrical insulation capability, due to its into carbon performance it is good the characteristics of cause its easily in spy
Electric trace deterioration occurs under conditions of fixed, tracking failure produces carbide in material surface, forms tungsten carbide/conductive path, meeting when serious
Cause short circuit, damage electric component.PPE another deficiency is that oil resistivity and solvent resistance (such as halogenated hydrocarbons, aromatic hydrocarbons) are poor, this limit
Its use in the case where these chemical environments may be contacted is made.Therefore, PPE relative discharge tracking index is improved
(Comparative Tracking Index), i.e. CTI, and improve its chemical resistance, for expanding PPE composites in electricity
The application of sub- electric field is significant.
Chinese patent application CN 105985624 discloses a kind of effective material for oil field flexibility collection petroleum pipeline transport layer
Material and preparation method thereof.It is constituted in percentage by weight, including ethylene-vinyl alcohol copolymer 5~15%；Nylon 10~
30%；Polyphenylene oxide 20~60%；Compatilizer 5~15%；Toughener 4~8%.Although the standby composite of the patent system has height
Warm tensile strength is high, good, the good pliability of oil resistivity and the features such as excellent processing characteristics, but its do not carry out it is flame-retardant modified,
Patent does not also carry out research explanation to the CTI of material simultaneously.
Chinese patent application CN 105602229A disclose a kind of Polyphenyl ether/polyamide alloy material for preparing fuel tank cap.
It is constituted in percentage by weight, including polyphenylene oxide 40~80%；Polyamide 20~60%；Polystyrene 3~15%；Function
Master batch 3~8%；Elastomer 1~10%；Graft 5~15%；Fire retardant 1~15%；Antioxidant 0.1~0.6%.The material
Although with excellent fire resistance and oil resistance, the heat resistance of material is relatively low, and equally the CTI of material is not carried out
Research.
Chinese patent application CN 103160108A disclose a kind of halogen-free fire-retardant polyphenyl ether/nylon 6 mixing alloy and its system
Preparation Method and application.It is constituted in percentage by weight, including polyphenylene oxide 20~80%；Nylon 6 10~40%；Compatilizer 5
~35%；The toughener 5~15% of fire retardant 5~20%；Antioxidant 0.2~0.5%；Lubricant 0.2~0.7%；Auxiliary agent 3~
35.5%.Although the material is with good fire resistance and higher heat resistance, not to the oil resistivity and CTI of material
Studied.
The content of the invention
In place of shortcoming and defect to solve prior art, primary and foremost purpose of the invention is to provide a kind of oil resistant high CTI
Value halogen free flame-retardant polyphenylene oxide composite material.The composite has excellent heat resistance energy, excellent oil resistance, excellent anti-electric-mark
Destructive characteristics and fire resistance, can be used for higher to the above performance requirement association area such as electric.
Another object of the present invention is to provide the preparation side of above-mentioned oil resistant high CTI value halogen free flame-retardant polyphenylene oxide composite material
Method.
The object of the invention is achieved through the following technical solutions：
A kind of oil resistant high CTI value halogen free flame-retardant polyphenylene oxide composite material, the composite is by polyphenylene oxide (PPE), nylon66 fiber
(PA66), halogen-free flame retardants, compatilizer, toughener, glass, antioxidant and lubricant composition, calculated in weight percent, each group
Divide consumption as follows：
Preferably, described PPE intrinsic viscosities are 0.35~0.65dL/g (25 DEG C of chloroforms).Less than (25 DEG C of 0.35dL/g
Chloroform) polyphenylene oxide molecular weight it is too low, influence the mechanical performance and heat resistance of material, and higher than 0.65dL/g (25 DEG C of chloroforms)
Although when mechanical performance and heat resistance it is good, due to its poor fluidity, be unfavorable for processing.
Preferably, described PA66, its intrinsic viscosity is 2.0~3.4.Intrinsic viscosity is less than 2.0 PA66 molecular weight mistakes
Low, material mechanical performance is poor, and intrinsic viscosity is higher than 3.4 PA66 poor fluidities, brings processing difficulties.
Preferably, the halogen-free flame retardants is red phosphor masterbatch；The red phosphor masterbatch is preferably by 40%~60% (weight
Amount), the red phosphorus of 500~1500 mesh first pass through stabilizer, low-molecular-weight wax cladding after obtained again with the extruding pelletization of nylon 6.
Preferably, the compatilizer is PPE-g-MAH (polyphenylene oxide grafted maleic anhydride).Contain PPE-g-MAH one end
With the extraordinary resin of PPE compatibilities, the other end contain can with nylon66 fiber strand amino react MAH, can improve PA66 with
PPE compatibility, plays more preferable compatible role.
Preferably, the toughener is POE-g-MAH (polyethylene glycol oxide grafted maleic anhydride).
Preferably, described glass fibre (glass) is alkali-free glass fibre, and 7~17 μm of filament diameter, chopped length 3
~24mm.The fiber that diameter is less than 7 μm prepares difficulty, and is easily worn and torn during composite processing, and loss of strength is very
Greatly；Diameter be more than 17 μm of glass can influence and resin combination, the performance of same influence composite.In order to increase glass with
The adhesion of resin, glass surface is handled using silane coupler.
Preferably, described antioxidant is the compounding antioxidant system that hindered phenol and phosphite ester are constituted.
Preferably, described lubricant is pentaerythritol stearate (PETS).
In order to improve PPE composites CTI than relatively low, and the shortcoming of oil resistivity difference, while keeping good heat-resisting of PPE
Performance and anti-flammability, the present invention add PA66 and halogen-free flame retardants red phosphor masterbatch in PPE, while carrying out fiberglass reinforced.PA66
Addition can improve PPE processing characteristics, improve its CTI value and oil resistance.Red phosphor masterbatch flame retarding efficiency is high, while will not
Heat resistance and CTI to material are negatively affected.The addition of glass can also be significantly improved in addition to improving the intensity of material
The heat resistance and oil resistance of material.
A kind of preparation method for preparing above-mentioned oil resistant high CTI value halogen free flame-retardant polyphenylene oxide composite material, comprises the following steps：
PPE, PA66, halogen-free flame retardants, compatilizer, toughener, antioxidant and lubricant are added into mixer to mix, by mixed thing
Material adds extruder main feeding hopper, and in side, feeding hopper adds glass fibre, by double screw extruder extruding pelletization, and oil resistant is made
High CTI value halogen free flame-retardant polyphenylene oxide composite material.
Preferably, above-mentioned incorporation time is 3~5min；The rotating speed of double screw extruder is 300~500r/min, and temperature is
250~290 DEG C.
Compared with prior art, the present invention has advantages below and beneficial effect：
(1) PA66 is added, the oil resistance and CTI values of PPE composites can be significantly improved, PPE composites are expanded
Application in electric field；
(2) use red phosphor masterbatch for halogen-free flame retardants, its heat endurance is good, its high phosphorus content brings high flame retarding efficiency,
Being decreased obviously for PPE composite heat resistances will not be caused as other phosphoric acid ester halogen-free flame retardants simultaneously；
(3) fiberglass reinforced is carried out, the mechanical performance, heat resistance and oil resistance of material is greatly improved, PPE is expanded and is combined
The application of material.
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.
The embodiment of the present invention and comparative example are molded into the standard batten of test according to standard requirement and tested.Draw
Stretch test according to ISO527 standards, Izod notched impact strength according to ISO180 standards, heat distortion temperature test according to
ISO75-2 standards (1.8MPa), CTI is tested according to IEC60112 standards.Oil resistant testing standard is as follows：(1) tensile bars are put
It is placed in the closed glass jar equipped with No. 95 gasoline, batten is completely soaked in the oil；(2) vial that will be equipped with batten is placed
Tested 500 hours in 80 DEG C of constant temperature oven；(3) after the completion of Soak Test, wipe clean and be positioned over 23 DEG C after the oil stain of surface, it is wet
Extension test is carried out after 24 hours in the incubator of degree 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.Fire resistance is tested according to UL94 vertical combustion standards.
The raw material used in the embodiment of the present invention and comparative example is as follows：
Polyphenylene oxide：LXR045 [intrinsic viscosity 0.45dL/g (25 DEG C of chloroforms)] Lanxing Chemical New Material Co., Ltd.；
Nylon66 fiber：PA66EPR27 (intrinsic viscosity 2.7), China Shenma Group Co., Ltd.；
Halogen-free flame retardants：20450N3 (red phosphor masterbatch, red phosphorus content 50%, the carrier of nylon 6), Nantong meaning specialization work is limited
Company；
Compatilizer：CX-1 (PPE-g-MAH, grafting rate 1.0%), Japanese light extraction (Idemitsu) company；；
Toughener：FUSN493D (POE-g-MAH), Dupont (DuPont) company；
Glass ECS3014B：13 μm of filament diameter, chopped length 4.5mm, Chongqing Polycomp International Co., Ltd；
Antioxidant：Hindered phenol 1098 (N, N'- pairs-(3- (3,5- di-tert-butyl-hydroxy phenyl) propiono) hexamethylene diamine),
German BASF (Basf) company；Phosphite ester S-9228 (double (2,4-two cruel bases) pentaerythritol diphosphites), the U.S. is all
Good fortune (Dover) company；
Lubricant：PETS (pentaerythritol stearate), husky (Lonza) company of U.S. dragon.
Embodiment 1
A kind of preparation method of oil resistant high CTI value halogen free flame-retardant polyphenylene oxide composite material, comprises the following steps：
(1) original is weighed by the amount of PPE in table 1, PA66, halogen-free flame retardants, compatilizer, toughener, antioxidant and lubricant
Material；
(2) various raw materials are mixed into 5min in mixer, then adds extruder main feeding hopper, feeding hopper is added in side
Glass, passes through double screw extruder extruding pelletization.
The rotating speed of double screw extruder is 300r/min, and temperature is 250~290 DEG C.The oil resistant high CTI value halogen free resistance of gained
Combustion polyphenylene oxide composite material performance is shown in Table 2.
Embodiment 2
A kind of preparation method of oil resistant high CTI value halogen free flame-retardant polyphenylene oxide composite material, comprises the following steps：
(1) original is weighed by the amount of PPE in table 1, PA66, halogen-free flame retardants, compatilizer, toughener, antioxidant and lubricant
Material；
(2) various raw materials are mixed into 3min in mixer, then adds extruder main feeding hopper, feeding hopper is added in side
Glass, passes through double screw extruder extruding pelletization.
The rotating speed of double screw extruder is 500r/min, and temperature is 250~290 DEG C.The oil resistant high CTI value halogen free resistance of gained
Combustion polyphenylene oxide composite material performance is shown in Table 2.
Embodiment 3~4
Embodiment 3~4 is weighed after raw material by table 1 respectively, according to the method for embodiment 1 prepare oil resistant high CTI value without
Halogen flame-proof polyphenylene oxide composite material, the oil resistant high CTI value halogen free flame-retardant polyphenylene oxide composite material performance of gained is shown in Table 2.
Comparative example 1~5
Comparative example 1~5 is weighed after raw material according to table 3 respectively, is prepared and changed by the conventional method of existing polyphenylene oxide
Property polyphenylene oxide sample.The Noryl properties of sample detection of gained is shown in Table 4.
The composition of the oil resistant high CTI value halogen free flame-retardant polyphenylene oxide composite material of table 1
The embodiment performance detection of table 2
The composition of the comparative example polyphenylene oxide composite material of table 3
The comparative example performance detection of table 4
Off grade：Flame does not go out to burn to fixture always, fails to obtain Vertical Flame test grading.
By comparative example 1 as can be seen that the CTI of pure PPE resins is very low, only 200V, and added with PA66 each implementation
The CTI of example PPE composites is improved significantly.
The addition that can be seen that toughener FUSN493D by the comparison of comparative example 2 and embodiment 1 can significantly improve material
The toughness of material, this is due to that PA66 mobility is preferable, continuous phase structure is easily formed in system, using the efficient toughener of PA66
POE-g-MAH, can improve the impact resistance of whole system.
The addition that can be seen that fire retardant 20450N3 by the comparison of comparative example 3 and embodiment 2 can significantly improve PPE
The fire resistance of composite, fire resistance is changed into V0 from off grade, while will not be to the heat resistance and CTI bands of composite
Significantly negatively affect.
The addition that can be seen that glass by the comparison of comparative example 4 and embodiment 3 can not only significantly improve PPE and be combined
The heat resistance of material, can also improve its oil resistance.
The raising that can be seen that PA66 contents by the contrast of comparative example 5 and embodiment 4 can significantly improve PPE and be combined
Oil resistance, CTI values and the heat resistance of material, but can decline PPE fire resistance.
Above-described embodiment is preferably embodiment, but embodiments of the present invention are not by above-described embodiment of the invention
Limitation, other any Spirit Essences without departing from the present invention and the change made under principle, modification, replacement, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (10)
1. a kind of oil resistant high CTI value halogen free flame-retardant polyphenylene oxide composite material, it is characterised in that the composite by PPE,
PA66, halogen-free flame retardants, compatilizer, toughener, glass, antioxidant and lubricant composition, calculated in weight percent, each component
Consumption is as follows：
2. a kind of oil resistant high CTI value halogen free flame-retardant polyphenylene oxide composite material according to claim 1, it is characterised in that institute
The PPE intrinsic viscosities stated are 0.35~0.65dL/g.
3. a kind of oil resistant high CTI value halogen free flame-retardant polyphenylene oxide composite material according to claim 1, it is characterised in that institute
The PA66 stated, its intrinsic viscosity is 2.0~3.4.
4. a kind of oil resistant high CTI value halogen free flame-retardant polyphenylene oxide composite material according to claim 1, it is characterised in that institute
The halogen-free flame retardants stated is the red phosphor masterbatch of PA6 carriers.
5. a kind of oil resistant high CTI value halogen free flame-retardant polyphenylene oxide composite material according to claim 1, it is characterised in that institute
The compatilizer stated is PPE-g-MAH.
6. a kind of oil resistant high CTI value halogen free flame-retardant polyphenylene oxide composite material according to claim 1, it is characterised in that institute
The toughener stated is POE-g-MAH.
7. a kind of oil resistant high CTI value halogen free flame-retardant polyphenylene oxide composite material according to claim 1, it is characterised in that institute
The glass fibre stated is 7~17 μm of filament diameter, 3~24mm of chopped length alkali-free glass fibre.
8. a kind of oil resistant high CTI value halogen free flame-retardant polyphenylene oxide composite material according to claim 1, it is characterised in that institute
The antioxidant stated is the compounding antioxidant system that hindered phenol and phosphite ester are constituted；Described lubricant is pentaerythrite stearic acid
Ester.
9. the preparation method of the oil resistant high CTI value halogen free flame-retardant polyphenylene oxide composite material described in any one of claim 1 to 7, its
It is characterised by, comprises the following steps：By weight percentage, 25~40%PPE, 20~40%PA66,4~10% Halogens are hindered
Agent, 2~4% compatilizers, 3~8% toughener, 0.4~0.6% antioxidant, 0.4~0.6% 3~5min of mix lubricant are fired,
Mixed material is added into extruder main feeding hopper, 10~30% glass fibres is added from side feeding, passes through twin-screw extrusion
Machine extruding pelletization, is made oil resistant high CTI value halogen free flame-retardant polyphenylene oxide composite material.
10. the preparation method of oil resistant high CTI value halogen free flame-retardant polyphenylene oxide composite material according to claim 9, its feature
It is, the rotating speed of the double screw extruder is 300~500r/min, and temperature is 250~290 DEG C.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111117221A (en) * | 2019-12-10 | 2020-05-08 | 珠海格力绿色再生资源有限公司 | Low-water-absorption composite material and preparation method thereof |
| EP3663360A4 (en) * | 2017-08-03 | 2021-05-05 | Mitsubishi Engineering-Plastics Corporation | Resin composition and molded article |
| CN113717518A (en) * | 2021-09-22 | 2021-11-30 | 宁波华腾首研新材料有限公司 | Laser-markable halogen-free flame-retardant glass fiber reinforced alloy material and preparation method thereof |
| CN114561094A (en) * | 2022-01-25 | 2022-05-31 | 金发科技股份有限公司 | high-CTI halogen-free flame-retardant polyphenyl ether composition and preparation method and application thereof |
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| CN103865256A (en) * | 2014-03-11 | 2014-06-18 | 广州市聚赛龙工程塑料有限公司 | Halogen-free flame retardant nylon 6 with high heat resistance as well as preparation method and application thereof |
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| CN102732020A (en) * | 2012-07-17 | 2012-10-17 | 上海日之升新技术发展有限公司 | Flame-retardant glass fiber reinforced polyamide (PA) 66/ poly-p-phenylene oxide (PPO) alloy composition and preparation method thereof |
| CN103865256A (en) * | 2014-03-11 | 2014-06-18 | 广州市聚赛龙工程塑料有限公司 | Halogen-free flame retardant nylon 6 with high heat resistance as well as preparation method and application thereof |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| EP3663360A4 (en) * | 2017-08-03 | 2021-05-05 | Mitsubishi Engineering-Plastics Corporation | Resin composition and molded article |
| CN111117221A (en) * | 2019-12-10 | 2020-05-08 | 珠海格力绿色再生资源有限公司 | Low-water-absorption composite material and preparation method thereof |
| CN113717518A (en) * | 2021-09-22 | 2021-11-30 | 宁波华腾首研新材料有限公司 | Laser-markable halogen-free flame-retardant glass fiber reinforced alloy material and preparation method thereof |
| CN114561094A (en) * | 2022-01-25 | 2022-05-31 | 金发科技股份有限公司 | high-CTI halogen-free flame-retardant polyphenyl ether composition and preparation method and application thereof |
| CN114561094B (en) * | 2022-01-25 | 2023-11-21 | 金发科技股份有限公司 | High CTI halogen-free flame-retardant polyphenyl ether composition, and preparation method and application thereof |
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