CN109135249A - A method of guaranteeing conductive polyphenyl ether composite materials property - Google Patents
A method of guaranteeing conductive polyphenyl ether composite materials property Download PDFInfo
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- CN109135249A CN109135249A CN201810984165.5A CN201810984165A CN109135249A CN 109135249 A CN109135249 A CN 109135249A CN 201810984165 A CN201810984165 A CN 201810984165A CN 109135249 A CN109135249 A CN 109135249A
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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
- C08L71/123—Polyphenylene oxides not modified by chemical after-treatment
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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
- C08K2201/001—Conductive additives
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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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- 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
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Abstract
The invention belongs to technical field of polymer material processing, more particularly to a kind of method for guaranteeing conductive polyphenyl ether composite materials property, including following raw material: 35-40 parts of polyphenylene oxide, 10-14 parts of isotactic polyphenylacetylene, 8-16 parts of modified materials, 1-3 parts of ground carbon fiber powder, 0.55-0.65 parts of compatilizer, 0.2-0.4 parts of antioxidant, 1-2 parts of dispersing agent.The present invention is had the advantage that in the present invention compared with prior art by handling hollow glass microballoon; it can be improved the compatibility of itself and polyphenylene oxide and isotactic polyphenylacetylene; the synergistic effect of each raw material; extend resistance to low temperature and high temperature resistance; and ground carbon fiber powder and modified materials act synergistically; the electric conductivity of polyphenylene oxide can be enhanced; and its mechanical property is made to keep preferable; extend its scope of application; it is strong to react controllability; products obtained therefrom performance is stablized, and has wider electric conductivity, is suitble to large-scale production.
Description
Technical field
The invention belongs to technical field of polymer material processing, and in particular to a kind of guarantee conductive polyphenyl ether composite material power
The method for learning performance.
Background technique
Polyphenylene oxide resin is a kind of macromolecule engineering plastics of the nonpolar linear structure containing phenyl ring on main chain, this knot
Structure imparts the good physical mechanical property of material, heat resistance and electric insulating quality, and hygroscopicity is low, intensity is high, dimensionally stable
Property is good, and creep resistant is best in all thermoplastic engineering plastics under high temperature, but pure polyphenylene oxide resin vitrifying degree is high,
Machine-shaping is difficult, energy consumption is excessive, promotes be limited in actual use, in the prior art by the way that PP, PS, PA and elastomer is added
Deng being modified to component, but it will affect the anti-flammability of polyphenylene oxide resin after the addition, in addition high molecular material volume resistivity
Greatly, a large amount of sight spots are easily gathered and to hamper product quality, existing application No. is 2016101428858 application documents public affairs
A kind of conductive flame-resistant polyphenylether is opened, conductive agent used is that one or more, fire retardant are during graphite, carbon black, carbon fiber or steel are fine
Microcapsule coated red phosphorus and nano aluminium oxide, wherein microcapsule coated red phosphorus prepares that products obtained therefrom stability is poor, and conductive agent
The mechanical property that will affect composite material is added, equally also limits its popularization and use.
Summary of the invention
The purpose of the present invention is being directed to existing problem, a kind of guarantee conductive polyphenyl ether composite materials property is provided
Method.
The present invention is achieved by the following technical solutions: a kind of side guaranteeing conductive polyphenyl ether composite materials property
Method, including the following contents:
(1) raw material preparation includes 35-40 parts of polyphenylene oxide, 10-14 parts of isotactic polyphenylacetylene, modified materials 8-16 by weight
Part, 1-3 parts of ground carbon fiber powder, 0.55-0.65 parts of compatilizer, 0.2-0.4 parts of antioxidant, 1-2 parts of dispersing agent；
(2) modified materials the preparation method comprises the following steps: by weight, taking 8-12 parts of hollow glass microballoon, 42-50 parts of toluene, alkene
0.4-0.8 parts of propyl glycidyl ether, 80 DEG C reflux 3-4 hours under magnetic stirring, by products therefrom centrifuge washing 2-5 times,
Solid powder A is obtained after drying；By 6-10 parts of solid powder A and it is equivalent to the ethyl alcohol of 20-30 times of its weight in the reaction vessel
40-50 parts of acrylic acid first is added dropwise to letting nitrogen in and deoxidizing in reaction vessel under the conditions of ice-water bath in mixing under the conditions of magnetic agitation
Ester then heats to 45 DEG C and reacts 12 hours, after the completion rinse products therefrom with deionized water, obtains solid powder after dry
B after the completion disperses 18-22 parts of solid powder B ultrasound sound in the n,N-Dimethylformamide for being equivalent to 20-30 times of its weight,
0.2-0.6 parts of triethylamines, 1.8-2.4 parts of two phosphoryl chloride phosphorus oxychloride contracting melamines of pentaerythrite diphosphate ester, 4-6 parts of 2- acetyl oxygen are added
Base isobutyl acylbromide stirs 2-4 hours under the conditions of ice-water bath, is warming up to 35 DEG C of reactions 1-3 hours after the completion, dry after washing
To solid powder C；By C, 75-85 parts of n,N-Dimethylformamide of 18-22 parts of solid powders, 0.8-1.6 parts of phosphotungstic acids, 1.6-
Bis- [4- (4- the aminophenoxy phenyl)] propane of 2.2 parts of 2,2'- mix in the reaction vessel, letting nitrogen in and deoxidizing, are 120- in temperature
Be stirred to react under conditions of 130 DEG C 4-6 hours, after centrifuge washing dry to get；
(3) after mixing polyphenylene oxide, modified materials, blending granulation is carried out in double screw extruder, obtains intermediate pellet, then will
Intermediate pellet is mixed with surplus stock, is blended and is granulated to get product in double screw extruder.
As further improvement of these options, the crystallinity of the polyphenylene oxide is 50%, water absorption rate 0.06%, bending
Intensity is 129MPa, flame retardant rating V-0.
As further improvement of these options, the isotactic polyphenylacetylene is molten in toluene by load-type Titanium series catalyst
The stereospecfic polymerization that styrene is carried out in agent obtains the isotactic polyphenylacetylene that isotacticity is 98%.
As further improvement of these options, the partial size of the hollow glass microballoon is 10-60 μm, and wall thickness is
0.08-0.16g/cm³。
As further improvement of these options, the specification of the ground carbon fiber powder is 600 mesh, and bulk density is
300-570g/L, intensity >=4000MPa, water content≤0.8%, the resistivity are 1.5 × 10-3Ω·cm。
As further improvement of these options, the partial size of the modified materials is 20-60nm, and the water content of modified materials is
2-6wt%。
As further improvement of these options, the compatilizer is m- isopropenyl -2,2- dimethyl benzoyl isocyanide
Acid esters and maleic anhydride are mixed to get with weight ratio 12-16:1；Antioxidant is 2,2' methylene bis-(4- methyl-6-tert
Butylphenol)；Dispersing agent is stearmide, copper stearate, polyethylene glycol 200 are mixed to get with weight ratio 8:2-3:1.
As further improvement of these options, the step (3) is after mixing polyphenylene oxide, modified materials, in double spiral shells
In bar extruder, it is 305-315 DEG C in temperature and is granulated after mixings 40-60 minutes, the revolving speed of screw rod is 400-600 revs/min
Clock obtains intermediate pellet, then mixes intermediate pellet with surplus stock, in double screw extruder temperature be 265-285
It is granulated after being kneaded 20-30 minutes under conditions of DEG C, screw speed is 800-900 revs/min to get product.
The present invention has the advantage that compared with prior art by handling hollow glass microballoon in the present invention, energy
The compatibility of itself and polyphenylene oxide and isotactic polyphenylacetylene is enough improved, the synergistic effect of each raw material keeps gained composite material intermolecular
There are crosslinkings, have chemical stability, extend resistance to low temperature and high temperature resistance, its flame retardant property is made not ground carbon fiber
The influence of powder is tieed up, and ground carbon fiber powder and modified materials act synergistically, and can enhance the electric conductivity of polyphenylene oxide, and make its mechanical property
It being able to maintain preferably, extends its scope of application, reaction controllability is strong, and products obtained therefrom performance is stablized, there is wider electric conductivity,
It is suitble to large-scale production.
Specific embodiment
Detailed description of the preferred embodiments below.It should be understood that described herein specific
Embodiment is merely to illustrate and explain the present invention, and is not intended to restrict the invention.
The present invention will be described in detail by way of examples below.In following embodiment and control group, the polyphenyl
Ether is the polyphenylene oxide that the trade mark that Yuyao City rain profit plasticizing Co., Ltd provides is X333Z；The isotactic polyphenylacetylene, pentaerythrite
Bis- [4- (4- the aminophenoxy phenyl)] propane of two phosphoryl chloride phosphorus oxychloride contracting melamine of biphosphonate, 2,2'- are prepared by laboratory；It is used
Materials Styrene, toluene are provided by Jiangsu Dong Yi Chemical Co., Ltd.；The hollow glass microballoon is limited by Shanghai vibration rising sun chemical industry
Company provides；The allyl glycidyl ether, methyl acrylate, triethylamine are provided by Shanghai Dong Tu Import and Export Co., Ltd.；
The 2- acetoxyl group isobutyl acylbromide is provided by Dongguan City Wa Lixi Chemical Co., Ltd.；The phosphotungstic acid is by the safe prosperous chemical industry in Zhengzhou
Products Co., Ltd provides；
The ground carbon fiber powder is the product that the trade mark that Jiangsu Chuan Yu carbon fiber Science and Technology Ltd. provides is CJ-CF600；Institute
Antioxidant and compatilizer is stated to be provided by Shanghai Jian Bang industrial corporation.
Wherein, the crystallinity of the polyphenylene oxide is 50%, water absorption rate 0.06%, bending strength 129MPa, flame retardant rating
For V-0；The isotactic polyphenylacetylene is carried out the stereospecfic polymerization of styrene by load-type Titanium series catalyst in toluene solvant, is obtained
The isotactic polyphenylacetylene that isotacticity is 98%；The partial size of the hollow glass microballoon is 10-60 μm, wall thickness 0.08-0.16g/cm
³；The specification of the ground carbon fiber powder be 600 mesh, bulk density 300-570g/L, intensity >=4000MPa, water content≤
0.8%, the resistivity is 1.5 × 10-3Ω·cm；The partial size of the modified materials is 20-60nm, and the water content of modified materials is 2-
6wt%。
Embodiment 1
A method of guaranteeing conductive polyphenyl ether composite materials property, including the following contents:
(1) raw material preparation includes that 38 parts of polyphenylene oxide, 12 parts of modified materials, grinds carbon at 12 parts of isotactic polyphenylacetylene by weight
2 parts of fiber powder, 0.6 part of compatilizer, 0.3 part of antioxidant, 1.5 parts of dispersing agent；
(2) modified materials the preparation method comprises the following steps: by weight, take 10 parts of hollow glass microballoon, 46 parts of toluene, allyl contracting
It 0.6 part of water glycerin ether, flows back 3.5 hours for 80 DEG C under magnetic stirring, products therefrom centrifuge washing 4 times is consolidated after dry
Body powders A；8 parts of solid powder A are mixed in the reaction vessel with the ethyl alcohol for being equivalent to 25 times of its weight, under the conditions of ice-water bath
To letting nitrogen in and deoxidizing in reaction vessel, 45 parts of methyl acrylate is added dropwise under the conditions of magnetic agitation, then heats to 45 DEG C of reactions
12 hours, products therefrom is rinsed after the completion with deionized water, solid powder B is obtained after dry, after the completion by 20 parts of solid powder
Last B ultrasound sound is scattered in the n,N-Dimethylformamide for being equivalent to 25 times of its weight, and 0.4 part of triethylamine, 2.1 parts of Ji Wusi is added
Two phosphoryl chloride phosphorus oxychloride contracting melamine of alcohol biphosphonate, 5 parts of 2- acetoxyl group isobutyl acylbromides, are stirred 3 hours under the conditions of ice-water bath, complete
It is warming up to 35 DEG C after to react 2 hours, solid powder C is dried to obtain after washing；By 20 parts of solid powder C, 80 parts of N, N- diformazan
Bis- [4- (4- the aminophenoxy phenyl)] propane of base formamide, 1.2 parts of phosphotungstic acids, 1.9 parts of 2,2'- mix in the reaction vessel,
Letting nitrogen in and deoxidizing, temperature be 125 DEG C under conditions of be stirred to react 5 hours, after centrifuge washing dry to get；
(3) it after mixing polyphenylene oxide, modified materials, in double screw extruder, is made after temperature is 310 DEG C of mixings 50 minutes
Grain, the revolving speed of screw rod are 500 revs/min, obtain intermediate pellet, then mix intermediate pellet with surplus stock, in twin-screw
It is granulated after being kneaded 25 minutes under conditions of temperature is 275 DEG C in extruder, screw speed is 850 revs/min to get product.
Wherein, the compatilizer is m- isopropenyl -2,2- dimethyl benzoyl isocyanates and maleic anhydride with weight
Amount is mixed to get than 14:1；Antioxidant is 2,2' methylene bis-(4- methyl-6-tert-butylphenol)；Dispersing agent is stearoyl
Amine, copper stearate, polyethylene glycol 200 are mixed to get with weight ratio 8:2.5:1.
Embodiment 2
A method of guaranteeing conductive polyphenyl ether composite materials property, including the following contents:
(1) raw material preparation includes that 35 parts of polyphenylene oxide, 8 parts of modified materials, grinds carbon fiber at 14 parts of isotactic polyphenylacetylene by weight
Tie up 3 parts of powder, 0.55 part of compatilizer, 0.4 part of antioxidant, 2 parts of dispersing agent；
(2) modified materials the preparation method comprises the following steps: by weight, take 8 parts of hollow glass microballoon, 42 parts of toluene, allyl contracting
It 0.4 part of water glycerin ether, flows back 3 hours for 80 DEG C under magnetic stirring, by products therefrom centrifuge washing 2 times, obtains solid after dry
Powders A；10 parts of solid powder A are mixed in the reaction vessel with the ethyl alcohol for being equivalent to 30 times of its weight, under the conditions of ice-water bath
To letting nitrogen in and deoxidizing in reaction vessel, 50 parts of methyl acrylate is added dropwise under the conditions of magnetic agitation, then heats to 45 DEG C of reactions
12 hours, products therefrom is rinsed after the completion with deionized water, solid powder B is obtained after dry, after the completion by 22 parts of solid powder
Last B ultrasound sound is scattered in the n,N-Dimethylformamide for being equivalent to 30 times of its weight, and 0.2 part of triethylamine, 2.4 parts of Ji Wusi is added
Two phosphoryl chloride phosphorus oxychloride contracting melamine of alcohol biphosphonate, 6 parts of 2- acetoxyl group isobutyl acylbromides, are stirred 2 hours under the conditions of ice-water bath, complete
It is warming up to 35 DEG C after to react 3 hours, solid powder C is dried to obtain after washing；By 18 parts of solid powder C, 85 parts of N, N- diformazan
Bis- [4- (4- the aminophenoxy phenyl)] propane of base formamide, 0.8 part of phosphotungstic acid, 2.2 parts of 2,2'- mix in the reaction vessel,
Letting nitrogen in and deoxidizing, temperature be 130 DEG C under conditions of be stirred to react 6 hours, after centrifuge washing dry to get；
It (3) is that 315 DEG C of mixings are made after sixty minutes in temperature in double screw extruder after mixing polyphenylene oxide, modified materials
Grain, the revolving speed of screw rod are 400 revs/min, obtain intermediate pellet, then mix intermediate pellet with surplus stock, in twin-screw
It is granulated after being kneaded 30 minutes under conditions of temperature is 285 DEG C in extruder, screw speed is 900 revs/min to get product.
Wherein, the compatilizer is m- isopropenyl -2,2- dimethyl benzoyl isocyanates and maleic anhydride with weight
Amount is mixed to get than 16:1；Antioxidant is 2,2' methylene bis-(4- methyl-6-tert-butylphenol)；Dispersing agent is stearoyl
Amine, copper stearate, polyethylene glycol 200 are mixed to get with weight ratio 8:3:1.
Embodiment 3
A method of guaranteeing conductive polyphenyl ether composite materials property, including the following contents:
(1) raw material preparation includes that 40 parts of polyphenylene oxide, 16 parts of modified materials, grinds carbon at 10 parts of isotactic polyphenylacetylene by weight
1 part of fiber powder, 0.65 part of compatilizer, 0.2 part of antioxidant, 1 part of dispersing agent；
(2) modified materials the preparation method comprises the following steps: by weight, take 12 parts of hollow glass microballoon, 50 parts of toluene, allyl contracting
It 0.8 part of water glycerin ether, flows back 4 hours for 80 DEG C under magnetic stirring, by products therefrom centrifuge washing 5 times, obtains solid after dry
Powders A；6 parts of solid powder A are mixed in the reaction vessel with the ethyl alcohol for being equivalent to 20 times of its weight, it is right under the conditions of ice-water bath
40 parts of methyl acrylate is added dropwise in letting nitrogen in and deoxidizing in reaction vessel under the conditions of magnetic agitation, then heats to 45 DEG C of reactions 12
Hour, products therefrom is rinsed with deionized water after the completion, solid powder B is obtained after dry, after the completion by 18 parts of solid powder B
0.6 part of triethylamine, 1.8 parts of pentaerythrites is added in the n,N-Dimethylformamide for being equivalent to 20 times of its weight in ultrasonic disperse
Two phosphoryl chloride phosphorus oxychloride contracting melamine of biphosphonate, 4 parts of 2- acetoxyl group isobutyl acylbromides, are stirred 4 hours under the conditions of ice-water bath, are completed
After be warming up to 35 DEG C react 1 hour, solid powder C is dried to obtain after washing；By 22 parts of solid powder C, 75 parts of N, N- dimethyl
Bis- [4- (4- the aminophenoxy phenyl)] propane of formamide, 1.6 parts of phosphotungstic acids, 1.6 parts of 2,2'- mix in the reaction vessel, lead to
Nitrogen deoxygenation, temperature be 120 DEG C under conditions of be stirred to react 4 hours, after centrifuge washing dry to get；
It (3) is that 305 DEG C of mixings are made after forty minutes in temperature in double screw extruder after mixing polyphenylene oxide, modified materials
Grain, the revolving speed of screw rod are 600 revs/min, obtain intermediate pellet, then mix intermediate pellet with surplus stock, in twin-screw
It is kneaded under conditions of temperature is 265 DEG C in extruder and is granulated after twenty minutes, screw speed is 800 revs/min to get product.
Wherein, the compatilizer is m- isopropenyl -2,2- dimethyl benzoyl isocyanates and maleic anhydride with weight
Amount is mixed to get than 12:1；Antioxidant is 2,2' methylene bis-(4- methyl-6-tert-butylphenol)；Dispersing agent is stearoyl
Amine, copper stearate, polyethylene glycol 200 are mixed to get with weight ratio 8:2:1.
Embodiment 4
Conductive polyphenyl ether composite material is prepared according to method in embodiment 1, except that isotactic polyphenylacetylene such as replaces at the weight
The polyphenylene oxide of amount；
Embodiment 5
Conductive polyphenyl ether composite material is prepared according to method in embodiment 1, except that isotactic polyphenylacetylene such as replaces at the weight
The polyolefin of amount；
Embodiment 6
Conductive polyphenyl ether composite material is prepared according to method in embodiment 1, except that isotactic polyphenylacetylene such as replaces at the weight
The syndiotactic polytyrene of amount；
Embodiment 7
Conductive polyphenyl ether composite material is prepared according to method in embodiment 1, except that being that 600 purposes grind carbon fiber by specification
Dimension powder replace with etc. weight specification be 200 mesh ground carbon fiber powder；
Embodiment 8
Conductive polyphenyl ether composite material is prepared according to method in embodiment 1, except that modified materials such as are replaced at the weight
Hollow glass microballoon；
Embodiment 9
Conductive polyphenyl ether composite material is prepared according to method in embodiment 1, except that being free of ground carbon fiber powder；
Embodiment 10
Conductive polyphenyl ether composite material is prepared according to method in embodiment 1, except that the parts by weight of ground carbon fiber powder are 5
Part；
Embodiment 11
Conductive polyphenyl ether composite material is prepared according to method in embodiment 1, except that the parts by weight of modified materials are 5 parts；
Embodiment 12
Conductive polyphenyl ether composite material is prepared according to method in embodiment 1, except that compatilizer is maleic anhydride；
Performance detection is carried out to conductive polyphenyl ether composite material prepared by each group, CMT6104 type universal electrical is selected to stretch examination
Test machine testing tensile strength；XJV5.5 type Izodtest instrument is selected to detect impact strength；Select the thermal change of XWB-300A type
Shape temperature-indicating instrument detects heat distortion temperature (1.82MPa)；Select U1231A type multimeter detection specific volume performance；Select ZC-90F
Type high resistant instrument detection resistance；SHJ-36 type double screw extruder is selected to prepare composite material；The length of the composite material is
20cm, width 10cm, with a thickness of 2cm.
Wherein, Specific volume resistivities (SPV)=measurement resistance × width × thickness ÷ length；
The performance of each group composite material is detected, following result is obtained:
Table 1
| Group | Tensile strength (MPa) | Bending strength (MPa) | Bending modulus (MPa) | Notch impact strength (KJ/m2) | Heat distortion temperature (DEG C) | SPV(k Ω cm) |
| Embodiment 1 | 67.9 | 78.2 | 2568 | 84 | 186 | 0.92 |
| Embodiment 2 | 68.4 | 78.8 | 2574 | 82 | 189 | 0.75 |
| Embodiment 3 | 68.2 | 78.5 | 2571 | 83 | 186 | 0.86 |
| Embodiment 4 | 57.8 | 65.9 | 1876 | 87 | 149 | 9.25 |
| Embodiment 5 | 63.5 | 76.4 | 2395 | 92 | 143 | 10.85 |
| Embodiment 6 | 65.8 | 76.9 | 2457 | 88 | 156 | 7.49 |
| Embodiment 7 | 63.2 | 76.1 | 2374 | 93 | 184 | 0.36 |
| Embodiment 8 | 49.6 | 53.7 | 1285 | 74 | 128 | 18.75 |
| Embodiment 9 | 68.5 | 80.5 | 2582 | 82 | 172 | 254.29 |
| Embodiment 10 | 60.2 | 69.8 | 2296 | 78 | 198 | 0.85 |
| Embodiment 11 | 62.4 | 72.3 | 2384 | 86 | 135 | 43.56 |
| Embodiment 12 | 63.7 | 76.8 | 2398 | 91 | 186 | 0.95 |
As data in table 1 can be seen that in the present invention obtained by Compound Material Engineering intensity it is preferable, have stronger heat-resistant deforming
Stability, notch impact strength are kept preferably, and reduction is less, and electric conductivity is promoted obviously, and modified materials and ground carbon fiber powder are assisted
Same-action can enhance electric conductivity, and ground carbon fiber powder dosage is excessive, then will affect mechanical property, and modified materials are to composite material
Effect on thermal it is obvious, in compatilizer m- isopropenyl -2,2- dimethyl benzoyl isocyanates facilitate enhance composite wood
The mechanical strength of material.
Claims (8)
1. a kind of method for guaranteeing conductive polyphenyl ether composite materials property, which is characterized in that including the following contents:
(1) raw material preparation includes 35-40 parts of polyphenylene oxide, 10-14 parts of isotactic polyphenylacetylene, modified materials 8-16 by weight
Part, 1-3 parts of ground carbon fiber powder, 0.55-0.65 parts of compatilizer, 0.2-0.4 parts of antioxidant, 1-2 parts of dispersing agent；
(2) modified materials the preparation method comprises the following steps: by weight, taking 8-12 parts of hollow glass microballoon, 42-50 parts of toluene, alkene
0.4-0.8 parts of propyl glycidyl ether, 80 DEG C reflux 3-4 hours under magnetic stirring, by products therefrom centrifuge washing 2-5 times,
Solid powder A is obtained after drying；By 6-10 parts of solid powder A and it is equivalent to the ethyl alcohol of 20-30 times of its weight in the reaction vessel
40-50 parts of acrylic acid first is added dropwise to letting nitrogen in and deoxidizing in reaction vessel under the conditions of ice-water bath in mixing under the conditions of magnetic agitation
Ester then heats to 45 DEG C and reacts 12 hours, after the completion rinse products therefrom with deionized water, obtains solid powder after dry
B after the completion disperses 18-22 parts of solid powder B ultrasound sound in the n,N-Dimethylformamide for being equivalent to 20-30 times of its weight,
0.2-0.6 parts of triethylamines, 1.8-2.4 parts of two phosphoryl chloride phosphorus oxychloride contracting melamines of pentaerythrite diphosphate ester, 4-6 parts of 2- acetyl oxygen are added
Base isobutyl acylbromide stirs 2-4 hours under the conditions of ice-water bath, is warming up to 35 DEG C of reactions 1-3 hours after the completion, dry after washing
To solid powder C；By C, 75-85 parts of n,N-Dimethylformamide of 18-22 parts of solid powders, 0.8-1.6 parts of phosphotungstic acids, 1.6-
Bis- [4- (4- the aminophenoxy phenyl)] propane of 2.2 parts of 2,2'- mix in the reaction vessel, letting nitrogen in and deoxidizing, are 120- in temperature
Be stirred to react under conditions of 130 DEG C 4-6 hours, after centrifuge washing dry to get；
(3) after mixing polyphenylene oxide, modified materials, blending granulation is carried out in double screw extruder, obtains intermediate pellet, then will
Intermediate pellet is mixed with surplus stock, is blended and is granulated to get product in double screw extruder.
2. a kind of method for guaranteeing conductive polyphenyl ether composite materials property as described in claim 1, which is characterized in that described
The crystallinity of polyphenylene oxide is 50%, water absorption rate 0.06%, bending strength 129MPa, flame retardant rating V-0.
3. a kind of method for guaranteeing conductive polyphenyl ether composite materials property as described in claim 1, which is characterized in that described
Isotactic polyphenylacetylene is carried out the stereospecfic polymerization of styrene by load-type Titanium series catalyst in toluene solvant, and obtaining isotacticity is
98% isotactic polyphenylacetylene.
4. a kind of method for guaranteeing conductive polyphenyl ether composite materials property as described in claim 1, which is characterized in that described
The partial size of hollow glass microballoon is 10-60 μm, wall thickness 0.08-0.16g/cm3.
5. a kind of method for guaranteeing conductive polyphenyl ether composite materials property as described in claim 1, which is characterized in that described
The specification of ground carbon fiber powder is 600 mesh, bulk density 300-570g/L, intensity >=4000MPa, water content≤0.8%, institute
Stating resistivity is 1.5 × 10-3Ω·cm。
6. a kind of method for guaranteeing conductive polyphenyl ether composite materials property as described in claim 1, which is characterized in that described
The partial size of modified materials is 20-60nm, and the water content of modified materials is 2-6wt%.
7. a kind of method for guaranteeing conductive polyphenyl ether composite materials property as described in claim 1, which is characterized in that described
Compatilizer is that m- isopropenyl -2,2- dimethyl benzoyl isocyanates is mixed with maleic anhydride with weight ratio 12-16:1
It arrives；Antioxidant is 2,2' methylene bis-(4- methyl-6-tert-butylphenol)；Dispersing agent is stearmide, copper stearate, poly- second
Glycol 200 is mixed to get with weight ratio 8:2-3:1.
8. a kind of method for guaranteeing conductive polyphenyl ether composite materials property as described in claim 1, which is characterized in that described
Step (3) is after mixing polyphenylene oxide, modified materials, is 305-315 DEG C of mixing 40-60 points in temperature in double screw extruder
It is granulated after clock, the revolving speed of screw rod is 400-600 revs/min, intermediate pellet is obtained, then by intermediate pellet and surplus stock
Mixing is granulated after being kneaded 20-30 minutes under conditions of temperature is 265-285 DEG C in double screw extruder, and screw speed is
800-900 revs/min to get product.
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| CN201810984165.5A CN109135249A (en) | 2018-08-28 | 2018-08-28 | A method of guaranteeing conductive polyphenyl ether composite materials property |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111117203A (en) * | 2019-12-12 | 2020-05-08 | 上海普利特伴泰材料科技有限公司 | Conductive, high-mechanical-property and low-warpage fiber-reinforced polyphenyl ether composite material and preparation method thereof |
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| KR20110109594A (en) * | 2010-03-31 | 2011-10-06 | 현대이피 주식회사 | Glassfiber reinforced polyphenylene ether resin composition |
| CN103421296A (en) * | 2012-05-23 | 2013-12-04 | 上海杰事杰新材料(集团)股份有限公司 | PPO/PS blend alloy material and preparation method thereof |
| CN103421298A (en) * | 2012-05-23 | 2013-12-04 | 上海杰事杰新材料(集团)股份有限公司 | Polyphenyl ether / polystyrene blending alloy material and preparation method thereof |
| CN104130597A (en) * | 2014-07-08 | 2014-11-05 | 上海海事大学 | Hollow glass micro-spheres surface modification method |
| CN107602919A (en) * | 2017-09-22 | 2018-01-19 | 郑州圣莱特空心微珠新材料有限公司 | The method of modifying and gained of hollow glass microbead are modified the method that hollow glass microbead is used to prepare starch or composite membrane of polyvinyl alcohol |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| KR20110109594A (en) * | 2010-03-31 | 2011-10-06 | 현대이피 주식회사 | Glassfiber reinforced polyphenylene ether resin composition |
| CN103421296A (en) * | 2012-05-23 | 2013-12-04 | 上海杰事杰新材料(集团)股份有限公司 | PPO/PS blend alloy material and preparation method thereof |
| CN103421298A (en) * | 2012-05-23 | 2013-12-04 | 上海杰事杰新材料(集团)股份有限公司 | Polyphenyl ether / polystyrene blending alloy material and preparation method thereof |
| CN104130597A (en) * | 2014-07-08 | 2014-11-05 | 上海海事大学 | Hollow glass micro-spheres surface modification method |
| CN107602919A (en) * | 2017-09-22 | 2018-01-19 | 郑州圣莱特空心微珠新材料有限公司 | The method of modifying and gained of hollow glass microbead are modified the method that hollow glass microbead is used to prepare starch or composite membrane of polyvinyl alcohol |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111117203A (en) * | 2019-12-12 | 2020-05-08 | 上海普利特伴泰材料科技有限公司 | Conductive, high-mechanical-property and low-warpage fiber-reinforced polyphenyl ether composite material and preparation method thereof |
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