CN104592739A - PPO alloy material for ignition coil framework and preparation method thereof - Google Patents
PPO alloy material for ignition coil framework and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a PPO alloy material for an ignition coil framework and a preparation method thereof. The PPO alloy material is prepared from the following raw materials in parts by weight: 20-50 parts of polyphenyl ether PPO, 20-40 parts of polystyrene, 2-6 parts of a flexibilizer, 10-30 parts of glass fibers, 1-10 parts of an epoxy resin curing agent, 0.5-3 parts of maleic anhydride, 0.5-2 parts of a tert amine type epoxy resin curing accelerator and 0.2-1.5 parts of an antioxidant. The PPO alloy material disclosed by the invention has excellent epoxy resin cohesive property and excellent dimensional stability and aging resistance and can be applied to the coil framework in an engine ignition coil. The preparation process of the PPO alloy material disclosed by the invention is simple, convenient to operate and suitable for large-scale industrial production.
Description
Technical field
The invention belongs to polymeric material field, specifically, is a kind of ignition coil framework PPO alloy material and preparation method thereof.
Background technology
Engine igniting coil is that the group of engine igniting system wants integral part, and its effect is that the low voltage of automobile storage battery is promoted to the high-voltage that can cause the 20kv to 40kv of spark-discharge.Therefore wearing to prevent high-voltage down-firing coil to be electrically shocked, the insulation strength of increasing ignition coil component, usually adopting the method for encapsulated epoxy resin that each for spark coil parts are carried out insulation-encapsulated.If but spark coil parts material therefor can not form good bonding with epoxy resin, then the poorest between material and epoxy resin bonding point, minimum insulating point will be become, material breakdown or short circuit will be caused under high voltages, spark coil was lost efficacy.Further, in automobile ignition coil working process, due to constant ignition, coil heating, temperature reaches as high as more than 100 DEG C, after quitting work, and temperature can be reduced to air themperature again, winter cold district, temperature can be low to moderate subzero 20 DEG C even 30 DEG C, even lower.Spark coil uses under the environment that colds and heat succeed each other, because spark coil parts and epoxy resin embedding adhesive there are differences at coefficient of linear expansion, when alternating hot and cold time, between epoxy resin and spark coil parts, thermal stresses will be produced, cause spark coil to ftracture, cause spark coil to lose efficacy.If there is good cohesiveness between material and epoxy resin, then effectively can resists due to the thermal stresses between thermal shock generation material and epoxy resin, thus improve the work-ing life of spark coil.For these reasons, require, between ignition coil framework material and epoxy resin, there is good cohesiveness.
Polyphenylene oxide (chemical name poly-2,6-dimethyl-1,4-phenylate, be called for short PPO) be a kind of thermoplastic engineering plastic of excellent performance, there is higher mechanical property and thermotolerance, good stability of the dimension, rate of moisture absorption is low, specific inductivity and dielectric loss be not substantially by the impact of temperature, humidity and frequency, and its dielectric strength is best in engineering plastics, be a kind of engineering plastics of excellent electrical property, be specially adapted to make the ignition coil framework that need bear extra-high pressure for spark coil inside.In prior art, only has the consistency being improved PPO and epoxy resin in the course of the polymerization process by functionalization, and do epoxy resin modification with PPO, as patent CN102516532A, disclose a kind of preparation method of amination polyphenyl ether, it be at polymerization stage by PPO amination to improve the consistency of PPO and epoxy resin, but it prepares loaded down with trivial details, complicated operation, and this patent does not provide any proof PPO material and the cohesiveness of epoxy resin and the experimental data of ageing-resistant performance thereof simultaneously.Patent CN201210246089.0 discloses a kind of low dielectric high heat-resistant epoxy resin composition and method of making the same, it is by using polyphenylene oxide grafted maleic anhydride and reactive thinner to reduce the viscosity of system to solve polyphenylene oxide and epoxy resin compatibility problem, thus improve dielectric and the mechanical property of system, this patent does not relate to bonding and the ageing-resistant performance of PPO material and epoxy resin yet equally.Therefore, it is very necessary for researching and developing a kind of engine igniting coil skeleton PPO alloy material with good epoxy bond, excellent dimensional stabilizing and ageing-resistant performance.
Summary of the invention
The object of the invention is for deficiency of the prior art, a kind of ignition coil framework PPO alloy material is provided.
Of the present invention again one object be that a kind of preparation method of ignition coil framework PPO alloy material is provided.
For achieving the above object, the technical scheme that the present invention takes is:
A kind of ignition coil framework PPO alloy material, it is made up of the raw material of following weight part: polyphenylene oxide PPO 20-50 part, polystyrene 20-40 part, toughner 2-6 part, glass fibre 10-30 part, epoxy curing agent 1-10 part, maleic anhydride 0.5-3 part, tertiary amine-type epoxy resin curing accelerator 0.5-2 part, oxidation inhibitor 0.2-1.5 part.
Described polyphenylene oxide PPO limiting viscosity in 25 DEG C of chloroforms is 0.2-0.6dl/g.
Described polystyrene is General Purpose Polystyrenre GPPS or impact resistant polystyrene HIPS.
Described toughner be SBS, styrene-ethylene-butylene-styrene block copolymer, styrene ethylene-propylene-styrene type segmented copolymer one or more.
Described glass fibre is alkali-free roving glass fiber or chopped glass fiber.
Described epoxy curing agent is aromatic anhydride type epoxy curing agent.
Described aromatic anhydride type epoxy curing agent is Tetra hydro Phthalic anhydride, trimellitic anhydride, pyromellitic acid anhydride or Benzophenone carboxylic acid dianhydride.
Described tertiary amine-type epoxy resin curing accelerator is one or more in trolamine, xylidine, DMP-30 and methyl tetrahydro phthalic anhydride.
Described oxidation inhibitor is described oxidation inhibitor: oxidation inhibitor 24-44 (four (2, 4-di-tert-butylphenol)-4, 4'-xenyl diphosphites CAS:119345-01-6), irgasfos 168 (three [2.4-di-tert-butyl-phenyl] phosphorous acid ester CAS:31570-04-4), antioxidant 1010 (four [β-(3, 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester CAS:6683-19-8), carbon free radical scavenger HP136 (xylyl dibutyl benzofuranone CAS:181314-48-7) is by weight the compound being 1:0.5:0.5:0.3.
For realizing above-mentioned second object, the technical scheme that the present invention takes is:
A preparation method for ignition coil framework PPO alloy material, comprises the following steps:
(1) get the raw materials ready according to above arbitrary described component and parts by weight;
(2) polyphenylene oxide and maleic anhydride are put into high-speed mixer and mixing 2-5 minute, after added by twin screw extruder first paragraph cylindrical shell, blending extrusion, granulation;
(3) prepared by step (2) product, polystyrene, toughner, epoxy curing agent, tertiary amine-type epoxy resin curing accelerator, oxidation inhibitor puts into high-speed mixer and mixing 3-8 minute;
(4) added by twin-screw extrusion owner spout by each raw material of step (3), glass fibre is added by twin screw extruder middle and lower reaches; The rotating speed of described twin screw extruder is 180-600 rev/min, and temperature is 235-275 DEG C.
PPO and maleic anhydride, by the pre-treatment of reactive processing, are carried out reactive extrursion by the present invention, improve the content that PPO itself and epoxy resin have the maleic anhydride functional groups of response capacity.
In this alloy material production phase, introduce the acid anhydride type curing agent that can participate in epoxy resin cure reaction, improve the content that can react anhydride functional group in material further.
In this alloy material production phase, add the promotor that can promote that epoxy resin cure reacts, such promotor can promote the open loop of maleic anhydride functional groups, promotes the activity of maleic anhydride functional groups.
PPO alloy material of the present invention has more response type anhydride functional group compared with conventional P PO alloy material, can in the Curing Process of Epoxy of spark coil encapsulated phase with epoxy resin generation chemical action, thus make between material and epoxy resin, to form good interfacial adhesion.
The ignition coil framework PPO alloy material with epoxy resin with good adhesion of the present invention, has superior epoxy bond and excellent dimensional stability and ageing-resistant performance, can be applicable to the coil rack in engine igniting coil.
Advantage is:
1, the present invention is by reactive processing pre-treatment, and PPO and maleic anhydride are carried out reactive extrursion, improves the content that PPO itself and epoxy resin have the maleic anhydride functional groups of response capacity; In process of production, add acid anhydride type curing agent, promote the anhydride-functional mass contg that can react in material further; Add the promotor that can promote that epoxy resin cure reacts, promote the open loop of maleic anhydride functional groups, promote the activity of maleic anhydride functional groups.PPO alloy material of the present invention has more response type anhydride functional group, in the curing process with epoxy resin generation chemical action, makes to form excellent interfacial adhesion between material and epoxy resin.
2, oxidation inhibitor of the present invention is that oxidation inhibitor 24-44, irgasfos 168, antioxidant 1010 and carbon free trapping agent HP136 is composite in specific proportions, between each component, there is synergy, make material of the present invention have excellent ageing resistance, meet the ageing resistance requirement of engine periphery material.
3, PPO alloy material preparation technology of the present invention is simple, easy to operate, is more suitable for industrialization scale operation.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.Following examples will contribute to those skilled in the art and understand the present invention further, but not limit the present invention in any form.It should be pointed out that to those skilled in the art, without departing from the inventive concept of the premise, some distortion and improvement can also be made.These all belong to protection scope of the present invention.
Embodiment 1-6
(1) get the raw materials ready according to the component in table 1 and content;
(2) polyphenylene oxide and maleic anhydride are put into high-speed mixer and mixing 2-5 minute, after added by twin screw extruder first paragraph cylindrical shell, blending extrusion, granulation;
(3) prepared by step (2) product, polystyrene, toughner, epoxy curing agent, tertiary amine-type epoxy resin curing accelerator, oxidation inhibitor puts into high-speed mixer and mixing 3-8 minute;
(4) added by twin-screw extrusion owner spout by each raw material of step (3), glass fibre is added by twin screw extruder middle and lower reaches; The rotating speed of described twin screw extruder is 180 revs/min, and temperature is 235 DEG C.
It should be noted that:
In embodiment 1, screw rod rotating speed is 180 revs/min, and temperature is 235 DEG C; In embodiment 2, screw rod rotating speed is 500 revs/min, and temperature is 245 DEG C; In embodiment 3, screw rod rotating speed is 600 revs/min, and temperature is 255 DEG C; In embodiment 4, screw rod rotating speed is 400 revs/min, and temperature is 275 DEG C; In embodiment 5, screw rod rotating speed is 300 revs/min, and temperature is 255 DEG C; In embodiment 6, screw rod rotating speed is 400 revs/min, and temperature is 265 DEG C
In embodiment 1-6, polyphenylene oxide PPO used limiting viscosity in 25 DEG C of chloroforms is 0.2-0.6dl/g, selects the LXR045 that Ruicheng branch office of blue star Chinese workers novel material limited-liability company produces.
In embodiment 1-3, polystyrene used is impact resistant polystyrene HIPS, Shanghai match section petrochemical iy produced HIPS 622P; In embodiment 4-6, polystyrene (PS) used is General Purpose Polystyrenre GPPS.
In embodiment 1-2, toughner used is SBS, purchased from American Ke Teng company G1651; In embodiment 3-4, toughner used is styrene-ethylene-butylene-styrene block copolymer; In embodiment 5-6, toughner used is styrene ethylene-propylene-styrene block copolymer.
In embodiment 1-3, glass fibre used is alkali-free roving glass fiber, and megalith group produces 988A; In embodiment 4-6, glass fibre used is chopped glass fiber.
In embodiment 1-6, maleic anhydride molecule formula used is C
4h
2o
3, produced by dawn chemical plant, Nanjing.
In embodiment 1-3, epoxy curing agent used is Tetra hydro Phthalic anhydride, Shanghai Jiaohua Co., Ltd (CAS:85-44-9); Embodiment 4 epoxy curing agent used is trimellitic anhydride; Embodiment 5 epoxy curing agent used is pyromellitic acid anhydride; Embodiment 6 epoxy curing agent used is Benzophenone carboxylic acid dianhydride.
In embodiment 1-3, tertiary amine-type epoxy resin curing accelerator used is the DMP-30 (CAS:90-72-2) that mountain peak, Changzhou Chemical Co., Ltd. produces; Embodiment 4 tertiary amine-type epoxy resin curing accelerator used is trolamine; Embodiment 5 tertiary amine-type epoxy resin curing accelerator used is xylidine; Embodiment 6 tertiary amine-type epoxy resin curing accelerator used is methyl tetrahydro phthalic anhydride.
In embodiment 1-6, oxidation inhibitor used is oxidation inhibitor 24-44 (four (2, 4-di-tert-butylphenol)-4, 4'-xenyl diphosphites CAS:119345-01-6), irgasfos 168 (three [2.4-di-tert-butyl-phenyl] phosphorous acid ester CAS:31570-04-4), antioxidant 1010 (four [β-(3, 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester CAS:6683-19-8), carbon free radical scavenger HP136 (xylyl dibutyl benzofuranone CAS:181314-48-7) is by weight the compound being 1:0.5:0.5:0.3.
Table 1
Comparative example 1
(1) raw material is taken by following weight percent: polyphenylene oxide (PPO): 41.8%; HIPS 622P:30%; SEBS G1651:7%; Oxidation inhibitor: 1.2%.Put into high mixer and mix 6 minutes;
(2) added by twin-screw extrusion owner feeding by each raw material of step (1), 20% glass fibre 988A is added by twin screw extruder middle and lower reaches, and the rotating speed of twin screw extruder is 350 revs/min, and temperature is 255 DEG C.
Comparative example 2
(1) take PPO LXR04537.5% by following weight percent, maleic anhydride 2%, put into high-speed mixer and mixing 5 minutes, after added by twin screw extruder first paragraph cylindrical shell, blending extrusion, granulation;
(2) raw material is taken by following weight percent: the extrudate through step (1): 39.5%; HIPS 622P:30%; SEBS G1651:6%; Tetra hydro Phthalic anhydride: 3%; DMP-30:1.5%; Put into high mixer and mix 7 minutes;
(3) added by twin-screw extrusion owner feeding by each raw material of step (2), 20% glass fibre 988A is added by twin screw extruder middle and lower reaches, and the rotating speed of twin screw extruder is 450 revs/min, and temperature is 265 DEG C.
It should be noted that:
In comparative example 1, comparative example 2, polyphenylene oxide PPO used limiting viscosity in 25 DEG C of chloroforms is 0.2-0.6dl/g, selects the LXR045 that Ruicheng branch office of blue star Chinese workers novel material limited-liability company produces.
In comparative example 1, oxidation inhibitor used is oxidation inhibitor 24-44 (four (2,4-di-tert-butylphenol)-4,4'-xenyl diphosphites CAS:119345-01-6), irgasfos 168 (three [2.4-di-tert-butyl-phenyl] phosphorous acid ester CAS:31570-04-4), antioxidant 1010 (four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester CAS:6683-19-8), carbon free radical scavenger HP136 (xylyl dibutyl benzofuranone CAS:181314-48-7) be by weight being the compound of 1:0.5:0.5:0.3.
Comparative example 3
(1) raw material is taken by following weight percent: polyphenylene oxide PPO 38.7%, polystyrene 20%, toughner 6%, glass fibre 20%, epoxy curing agent 10%, maleic anhydride 3%, tertiary amine-type epoxy resin curing accelerator 2%, oxidation inhibitor 0.3%; Put into high mixer mixing 3-8 minute;
(2) added by twin-screw extrusion owner spout by each raw material of step (2), 20% glass fibre is added by twin screw extruder middle and lower reaches, and the rotating speed of twin screw extruder is 180 revs/min, and temperature is 235 DEG C.
Polyphenylene oxide PPO used limiting viscosity in 25 DEG C of chloroforms is 0.2-0.6dl/g, selects the LXR045 that Ruicheng branch office of blue star Chinese workers novel material limited-liability company produces; Polystyrene used is impact resistant polystyrene HIPS, Shanghai match section petrochemical iy produced HIPS 622P; Toughner used is SBS, purchased from American Ke Teng company G1651; Glass fibre used is alkali-free roving glass fiber, and megalith group produces 988A; Epoxy curing agent used is Tetra hydro Phthalic anhydride, Shanghai Jiaohua Co., Ltd (CAS:85-44-9); Tertiary amine-type epoxy resin curing accelerator used is the DMP-30 (CAS:90-72-2) that mountain peak, Changzhou Chemical Co., Ltd. produces; Oxidation inhibitor used is that the free trapping agent HP136 of oxidation inhibitor 24-44, irgasfos 168, antioxidant 1010 and carbon is by weight the compound for 1:0.5:0.5:0.3.
Comparative example 4
(1) raw material is taken by following weight percent: polyphenylene oxide PPO 38.7%, polystyrene 20%, toughner 6%, glass fibre 20%, epoxy curing agent 10%, maleic anhydride 3%, tertiary amine-type epoxy resin curing accelerator 2%, oxidation inhibitor 0.3%;
(2) polyphenylene oxide and maleic anhydride are put into high-speed mixer and mixing 2-5 minute, after added by twin screw extruder first paragraph cylindrical shell, blending extrusion, granulation;
(3) prepared by step (2) product, polystyrene, toughner, epoxy curing agent, tertiary amine-type epoxy resin curing accelerator, oxidation inhibitor puts into high-speed mixer and mixing 3-8 minute;
(4) added by twin-screw extrusion owner spout by each raw material of step (3), glass fibre is added by twin screw extruder middle and lower reaches; The rotating speed of described twin screw extruder is 180 revs/min, and temperature is 235 DEG C.
Polyphenylene oxide PPO used limiting viscosity in 25 DEG C of chloroforms is 0.2-0.6dl/g, selects the LXR045 that Ruicheng branch office of blue star Chinese workers novel material limited-liability company produces; Polystyrene used is impact resistant polystyrene HIPS, Shanghai match section petrochemical iy produced HIPS 622P; Toughner used is SBS, purchased from American Ke Teng company G1651; Glass fibre used is alkali-free roving glass fiber, and megalith group produces 988A; Epoxy curing agent used is Tetra hydro Phthalic anhydride, Shanghai Jiaohua Co., Ltd (CAS:85-44-9); Tertiary amine-type epoxy resin curing accelerator used is the DMP-30 (CAS:90-72-2) that mountain peak, Changzhou Chemical Co., Ltd. produces; Oxidation inhibitor used is oxidation inhibitor 24-44.
Material properties test: above-mentioned materials after 4 hours, is injection molded into standard batten with plastic injection molding machine in 90 DEG C of dryings in convection oven; The batten of injection formed is carried out performance test in the relative humidity of 50%, 23 DEG C of placements after at least 24 hours.Testing method is as follows:
Tensile strength: by ISO 527 method, draw speed 5mm/min;
Flexural strength: by ISO 178 method, trial speed 2mm/min;
Shock strength: by ISO 179 method, notch shock, simply supported beam;
Heat-drawn wire (HDT): by ISO 75 method, 1.82MPa load;
Epoxy bond is evaluated: according to ISO 4587 method, and epoxy resin adopts KYOCERA 1695, is warming up to 130 DEG C solidifies 3 hours again 90 DEG C of solidifications after 1.5 hours, and at 23 DEG C, place test after 24 hours.
Accelerated deterioration performance evaluation:
Tensile bars and notch shock batten are placed in 120 DEG C of convection oven, test performance after 1000 hours.F presses ISO 527 method, draw speed 5mm/min, the tensile strength of test material; By ISO 179 method, simply supported beam, the notched Izod impact strength of test material.
Carry out performance test comparison to product prepared by embodiment 1-6 and comparative example 1-4, result is as shown in table 2.
Table 2
As shown in Table 2, strengthen compared with PPO alloy material with comparative example 1 is common, the tensile shear strength with the PPO alloy material of good epoxy bond prepared by the present invention is significantly improved, the tensile shear strength of this alloy material promotes nearly one times, therefore PPO alloy material prepared by the present invention effectively improves the cohesiveness of PPO alloy and epoxy resin.Compared with comparative example 2, the antioxidant system of the present invention's application has excellent thermo oxidative aging performance, in comparative example 2, the performance of aging rear material obviously declines, fall is even more than 30%, and the fall adding this antioxidant system is all less than 25%, even only has 20%.
Ignition coil framework PPO alloy material of the present invention, has superior epoxy bond and excellent dimensional stability and ageing-resistant performance, can be applicable to the coil rack in engine igniting coil.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the prerequisite not departing from the inventive method; can also make some improvement and supplement, these improve and supplement and also should be considered as protection scope of the present invention.
Claims (10)
1. an ignition coil framework PPO alloy material, it is characterized in that, it is made up of the raw material of following weight part: polyphenylene oxide PPO 20-50 part, polystyrene 20-40 part, toughner 2-6 part, glass fibre 10-30 part, epoxy curing agent 1-10 part, maleic anhydride 0.5-3 part, tertiary amine-type epoxy resin curing accelerator 0.5-2 part, oxidation inhibitor 0.2-1.5 part.
2. PPO alloy material according to claim 1, is characterized in that, described polyphenylene oxide PPO limiting viscosity in 25 DEG C of chloroforms is 0.2-0.6dl/g.
3. PPO alloy material according to claim 1, is characterized in that, described polystyrene is General Purpose Polystyrenre GPPS or impact resistant polystyrene HIPS.
4. PPO alloy material according to claim 1, it is characterized in that, described toughner be SBS, styrene-ethylene-butylene-styrene block copolymer, styrene ethylene-propylene-styrene type segmented copolymer one or more.
5. PPO alloy material according to claim 1, is characterized in that, described glass fibre is alkali-free roving glass fiber or chopped glass fiber.
6. PPO alloy material according to claim 1, is characterized in that, described epoxy curing agent is aromatic anhydride type epoxy curing agent.
7. PPO alloy material according to claim 6, is characterized in that, described aromatic anhydride type epoxy curing agent is Tetra hydro Phthalic anhydride, trimellitic anhydride, pyromellitic acid anhydride or Benzophenone carboxylic acid dianhydride.
8. PPO alloy material according to claim 1, is characterized in that, described tertiary amine-type epoxy resin curing accelerator is one or more in trolamine, xylidine, DMP-30 and methyl tetrahydro phthalic anhydride.
9. PPO alloy material according to claim 1, is characterized in that, described oxidation inhibitor is that the free trapping agent HP136 of oxidation inhibitor 24-44, irgasfos 168, antioxidant 1010 and carbon is by weight the compound for 1:0.5:0.5:0.3.
10. an ignition coil framework preparation method for PPO alloy material, is characterized in that, comprise the following steps:
(1) get the raw materials ready according to the arbitrary described component of claim 1-9 and parts by weight;
(2) polyphenylene oxide and maleic anhydride are put into high-speed mixer and mixing 2-5 minute, after added by twin screw extruder first paragraph cylindrical shell, blending extrusion, granulation;
(3) prepared by step (2) product, polystyrene, toughner, epoxy curing agent, tertiary amine-type epoxy resin curing accelerator, oxidation inhibitor puts into high-speed mixer and mixing 3-8 minute;
(4) added by twin-screw extrusion owner spout by each raw material of step (3), glass fibre is added by twin screw extruder middle and lower reaches; The rotating speed of described twin screw extruder is 180-600 rev/min, and temperature is 235-275 DEG C.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102344663A (en) * | 2011-08-04 | 2012-02-08 | 南通中蓝工程塑胶有限公司 | Phase solvent suitable for reinforced polyphenylene oxide material |
| CN104119666A (en) * | 2014-07-14 | 2014-10-29 | 东莞市德诚塑化科技有限公司 | Conductive PPO material and preparation method thereof |
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| CN102344663A (en) * | 2011-08-04 | 2012-02-08 | 南通中蓝工程塑胶有限公司 | Phase solvent suitable for reinforced polyphenylene oxide material |
| CN104119666A (en) * | 2014-07-14 | 2014-10-29 | 东莞市德诚塑化科技有限公司 | Conductive PPO material and preparation method thereof |
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