CN103497500B - Polyphenylene oxide resin alloy material and preparation method and application thereof - Google Patents
Polyphenylene oxide resin alloy material and preparation method and application thereof Download PDFInfo
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Abstract
The invention belongs to the field of polymer alloy material and particularly relates to polyphenylene oxide resin alloy material for machining cases of electric car lithium batteries and a preparation method of the material. The polyphenylene oxide resin alloy material comprises, by weight, 40-60 parts of polyphenylene oxide resin, 20-60 parts of polystyrene resin, 1-3 parts of polyolefin, 1-8 parts of elastomer, 1-15 parts of flame retardant, 10-20 parts of glass fiber, 1-15 parts of graft body, 3-8 parts of functional master batch and 0.2-0.5 part of antioxidant. The process of the polyphenylene oxide resin alloy material is optimized through reasonable formula combination, and the problem that the cases of the electric car lithium batteries deforms and electrode connections of the batteries crack after long-term use of electric cars is solved.
Description
Technical field
The invention belongs to high molecule alloy material field, be specifically related to a kind of polyphenylether resin alloy material, its preparation method and application.
Background technology
Polyphenylene oxide resin has a lot of excellent performance, and such as mechanical property, hydrolysis, acid-alkali-corrosive-resisting, resistance toheat, dimensional stability etc., its product is employed for the fields such as electronic apparatus, automobile component, water treating equipment, chemical industry widely.At present, common polyphenylether resin alloy material, in battery case Application Areas, has certain advantage, and such as material itself has acid resistance, resistance toheat, dimensional stability and dielectric properties.But in use, have also discovered a lot of deficiency, such as electromobile travels for a long time and there will be battery case distortion, and cracking phenomena appears in the electrode connection of battery case.
Summary of the invention
Technical problem to be solved by this invention overcomes the deficiencies in the prior art, provides a kind of polyphenylether resin alloy material.
The present invention also provides a kind of preparation method of polyphenylether resin alloy material simultaneously.
For solving above technical problem, the present invention adopts following technical scheme:
Polyphenylether resin alloy material, with parts by weight, described polyphenylether resin alloy material comprises following recipe ingredient:
Wherein:
Described elastomerics is styrene-butadiene rubber(SBR), HSBR, ethylene propylene rubber, terpolymer EP rubber, polyacrylic rubber, Toughening Effect of Ethylene Copolymer Elastomer, polyisoprene elastomerics, 1, one or several the mixture in 2 polybutadiene elastomer;
Described grafting body is with the mixture of one or several in described polyphenylene oxide resin, polyvinyl resin, polyolefine, elastomerics for base material, and the grafts of described grafting body is one or several the mixture in diacetyl oxide, propionic anhydride, Succinic anhydried, MALEIC ANHYDRIDE, benzoyl oxide, Tetra hydro Phthalic anhydride.
In described functional agglomerate gross weight for 100%, described functional agglomerate comprises following recipe ingredient:
Wherein:
Described chirality mesoporous electro-conductive material is at least one in polyaniline, polypyrrole;
Described lubricant is at least one in silicone oil, stearic acid lubricant;
Described chiral inorganic mesoporous material is at least one in silicon-dioxide, titanium dioxide.
Described polyphenylene oxide resin is the mixture of one or both in the multipolymer of the polymkeric substance of 2,6-xylenol, 2,6-xylenols and 2,3,6-TMP, and its limiting viscosity is 0.2-0.6dl/g.
Described polystyrene resin is the mixture of the one or both in polystyrene, high-impact polystyrene.
Described polyolefine is one or several the mixture in polyethylene, polypropylene, ethylene propylene copolymer, polybutene, ethylene-butylene copolymer, ethene-unsaturated ester multipolymer.
Described fire retardant is phosphorus flame retardant and nitrogen based flame retardant is the compound system that 2 ~ 4:1 forms by weight, and wherein, described phosphorus flame retardant is the mixture of one or more in phosphate ester flame retardants, ammonium polyphosphate based flame retardant, inorganic phosphorus based flame retardant; Described nitrogen based flame retardant is the one in trimeric cyanamide, Dyhard RU 100 based flame retardant.
Described oxidation inhibitor is primary antioxidant and auxiliary antioxidant is the mixture that 1 ~ 3:1 forms by weight, wherein, described primary antioxidant is 3,5-di-tert-butyl-hydroxy phenyl propionic acid octadecyl, β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid octadecyl, 2, one or several the mixture in 2 methylene-biss (4-methyl-6-tert-butylphenol); Described auxiliary antioxidant is one or several the mixture in three (Isosorbide-5-Nitrae-di-tert-butyl-phenyl) phosphorous acid, two (2,4-di-tert-butyl-phenyl) pentaerythritol diphosphate, two (octadecyl) pentaerythritol diphosphate.
In the present invention, all described raw material, all by being purchased and/or taking known means to prepare, when not illustrated, all meets the requirement of stdn chemical product.
Polyphenylether resin alloy material of the present invention can be used for lithium ion battery of electric automobile shell.
The another technical scheme that the present invention takes is: a kind of preparation method of above-mentioned polyphenylether resin alloy material, comprises the following steps:
(1) prepare functional agglomerate: by the formula of described functional agglomerate, utilize twin screw extruder extruding pelletization, temperature controls to melt extrude under 260-300 DEG C of condition, and main frame revolution controls at 250-350RPM, and vacuum degree control is at 0.5-0.8MPa.
(2) polyphenylether resin alloy material is prepared: by the formula of described polyphenylether resin alloy material, first described polyolefine, elastomerics, fire retardant, grafting body, functional agglomerate, oxidation inhibitor are mixed formation mixture, then, after described polyphenylene oxide resin, described polystyrene resin, described mixture and described glass fibre being added from the different charging openings of twin screw extruder, melt extrude.
Due to the enforcement of technique scheme, the present invention compared with prior art tool has the following advantages:
Polyphenylether resin alloy material of the present invention, by with the use of polyphenylene oxide resin, polystyrene resin, polyolefine, elastomerics, fire retardant, grafting body, functional agglomerate, oxidation inhibitor, the usage ratio of reasonably optimizing above-mentioned raw materials, makes polyphenylether resin alloy material not easily deform, also not easily ftractures after being soaked by electrolytic solution simultaneously.This polyphenylether resin alloy material is applied to lithium ion battery of electric automobile shell, effectively can solve current electromobile under long-time use, casing of lithium ion battery deform and casing of lithium ion battery electrode connection occur cracking phenomenon, fully meet the service requirements of lithium ion battery of electric automobile shell.The preparation method of polyphenylether resin alloy material of the present invention is simple to operate, with low cost, productivity effect is high, and prepared polyphenylether resin alloy material not easily deforms, also not easily ftracture after being soaked by electrolytic solution, is suitable for suitability for industrialized production.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described.
Each raw material weight number is in table 1.The manufacturer of each raw material is:
Embodiment 1
The present embodiment adopt raw material and consumption see table 1, wherein:
Polyphenylene oxide resin: the polymkeric substance being selected from 2,6-xylenol, its limiting viscosity is 0.4dl/g;
Polystyrene resin: be selected from high-impact polystyrene;
Polyolefine: be made up of by weight for 2:1 polyethylene, polypropylene;
Elastomerics: be made up of by weight for 1:1 styrene-butadiene rubber(SBR), HSBR elastomerics;
Fire retardant: be made up of by weight for 3:1 phosphorus flame retardant and nitrogen based flame retardant, wherein, phosphorus flame retardant is phosphate ester flame retardants, and nitrogen based flame retardant is trimeric cyanamide;
The special alkali free glass fibre of glass fibre: PPO.
Grafting body: with polyphenylene oxide resin, polyvinyl resin, polyolefine by weight the mixture for 7:2:1 composition for base material, grafts is diacetyl oxide;
Oxidation inhibitor: be made up of by weight for 2:1 primary antioxidant and auxiliary antioxidant, wherein, primary antioxidant is 3,5-di-tert-butyl-hydroxy phenyl propionic acid octadecyl, auxiliary antioxidant is by three (1,4-di-tert-butyl-phenyl) phosphorous acid, two (2,4-di-tert-butyl-phenyl) pentaerythritol diphosphate by weight for 1:1 form;
Functional agglomerate: self-control, take polystyrene resin as base material, be loaded into chirality mesoporous electro-conductive material, lubricant, chiral inorganic mesoporous material formed jointly, by weight percentage, polyphenylene oxide resin accounts for 85%, chirality mesoporous electro-conductive material is that polypyrrole accounts for 5%, lubricant is that silicone oil accounts for 6%, chiral inorganic mesoporous material is that silicon-dioxide and titanium dioxide account for 4% by weight the mixture formed for 1:1.
The preparation process of polyphenylether resin alloy material is as follows:
(1) prepare functional agglomerate: by the formula of functional agglomerate, utilize twin screw extruder extruding pelletization, temperature controls to melt extrude under 260-300 DEG C of condition, and main frame revolution controls at 250-350RPM, and vacuum degree control is at 0.5-0.8MPa.
(2) polyphenylether resin alloy material is prepared: by formula, first polyolefine, elastomerics, fire retardant, grafting body, functional agglomerate, oxidation inhibitor are mixed formation mixture, then polyphenylene oxide resin is added from the first weightless charging opening, polystyrene resin adds from the second weight loss feeders mouth, mixture adds from the 3rd weight loss feeders mouth, glass fibre adds from side direction spout, through twin screw extruder plasticizing, melting, extrude, tie rod, cooling, pelletizing.Pellet is at gas blower drying oven 120 DEG C of dry 2-4h, and then test bars and goods are prepared in injection moulding.
Embodiment 2
The raw material that the present embodiment adopts and consumption are see table 1, and the raw material outside polyphenylene oxide resin, polystyrene resin, polyolefine is all identical with embodiment 1.
In this example, polyphenylene oxide resin: by the multipolymer of the polymkeric substance of 2,6-xylenol, 2,6-xylenols and 2,3,6-TMP by weight the mixture for 1:1 composition, its limiting viscosity is 0.6dl/g;
In this example, polystyrene resin: be made up of by weight for 1:1 polystyrene, high-impact polystyrene;
In this example, polyolefine: be made up of by weight for 3:1:1 polyethylene, ethylene propylene copolymer, polybutene;
In the present embodiment, the preparation method of polyphenylether resin alloy material, with embodiment 1, no longer repeats at this.
Embodiment 3
The raw material that the present embodiment adopts and consumption are see table 1, and the raw material outside elastomerics, fire retardant, functional agglomerate is all identical with embodiment 1.
In this example, elastomerics: be selected from styrene-butadiene rubber(SBR);
In this example, fire retardant: be made up of by weight for 4:1 phosphorus flame retardant and nitrogen based flame retardant, wherein, phosphorus flame retardant is ammonium polyphosphate based flame retardant, and nitrogen based flame retardant is trimeric cyanamide;
In this example, functional agglomerate: self-control, with polystyrene resin, elastomerics by weight for the mixture of 5:1 composition is for base material, be loaded into chirality mesoporous electro-conductive material, lubricant, chiral inorganic mesoporous material formed jointly, by weight percentage, base material accounts for 80%, chirality mesoporous electro-conductive material is that polyaniline accounts for 8%, lubricant is that silicone oil accounts for 6%, chiral inorganic mesoporous material is that silicon-dioxide accounts for 6%.
In the present embodiment, the preparation method of polyphenylether resin alloy material, with embodiment 1, no longer repeats.
Embodiment 4
The raw material that the present embodiment adopts and consumption are see table 1, and the raw material outside grafting body, oxidation inhibitor, functional agglomerate is all identical with embodiment 1.
In this example, grafting body: take polyvinyl resin as base material, grafts is made up of by weight for 1:1 benzoyl oxide, Tetra hydro Phthalic anhydride;
In this example, oxidation inhibitor: be made up of by weight for 3:1 primary antioxidant and auxiliary antioxidant, wherein, primary antioxidant is by β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid octadecyl, 2,2 methylene-biss (4-methyl-6-tert-butylphenol) are by weight being 1:1 composition, and auxiliary antioxidant is two (2,4-di-tert-butyl-phenyl) pentaerythritol diphosphate;
In this example, functional agglomerate: self-control, with polyolefine, elastomerics by weight for the mixture of 5:1 composition is for base material, be loaded into chirality mesoporous electro-conductive material, lubricant, chiral inorganic mesoporous material formed jointly, by weight percentage, base material accounts for 90%, chirality mesoporous electro-conductive material is that polyaniline accounts for 3%, lubricant is that silicone oil accounts for 2%, chiral inorganic mesoporous material is that silicon-dioxide accounts for 5%.
In this example, the preparation method of polyphenylether resin alloy material, with embodiment 1, no longer repeats.
Comparative example 1
This comparative example does not add grafting body and functional agglomerate when preparing polyphenylether resin alloy material, and all the other raw materials are identical with embodiment 1.
The preparation method of the polyphenylether resin alloy material of this comparative example is: by formula, first polyolefine, elastomerics, fire retardant, oxidation inhibitor are mixed formation mixture, then polyphenylene oxide resin is added from the first weightless charging opening, polystyrene resin adds from the second weight loss feeders mouth, mixture adds from the 3rd weight loss feeders mouth, glass fibre adds from side direction spout, through twin screw extruder plasticizing, melting, extrude, tie rod, cooling, pelletizing.Pellet is at gas blower drying oven 120 DEG C of dry 2-4h, and then test bars and goods are prepared in injection moulding.
The raw material weight number proportioning of table 1 embodiment 1 ~ 4, comparative example 1
| Component | Comparative example 1 | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 |
| Polyphenylene oxide resin | 46 | 52 | 48 | 43 | 40 |
| Polystyrene resin | 28.7 | 24.7 | 25.7 | 22.7 | 21.7 |
| Polyolefine | 1 | 1 | 1 | 1 | 1 |
| Elastomerics | 1 | 1 | 1 | 1 | 1 |
| Fire retardant | 8 | 6 | 7 | 9 | 11 |
| Glass fibre | 15 | 10 | 12 | 18 | 20 |
| Grafting body | 0 | 2 | 2 | 2 | 2 |
| Functional agglomerate | 0 | 3 | 3 | 3 | 3 |
| Oxidation inhibitor | 0.3 | 0.3 | 0.3 | 0.3 | 0.3 |
Composition properties test result in table 2 embodiment and comparative example
As can be seen from the performance test table of table 2, polyphenylether resin alloy material of the present invention not easily deforms, also not easily ftracture after being soaked by electrolytic solution.
The performance of composition in test and Evaluation operation example and comparative example by the following method.
(1) tensile strength
Described tensile strength is pressed ASTM D-638 and is tested.
(2) flexural strength
Described flexural strength is pressed ASTM D-790 and is tested.
(3) modulus in flexure
Described modulus in flexure is pressed ASTM D-790 and is tested
(4) notched Izod impact strength
Described notched Izod impact strength is pressed ASTM D-256 and is tested.
(5) heat-drawn wire
Described heat-drawn wire presses ASTM D-648 standard testing.
(6) shrinking percentage
Described shrinking percentage presses ASTM D-570 standard testing.
(7) flame retardant properties
Described flame retardant properties presses UL94 standard testing.
(8) material deformation test
The product of injection moulding to be positioned under room temperature after 24H, put into 120 DEG C of baking oven 24H, static to room temperature, put into-30 DEG C of refrigerator 24H again, then leave standstill to room temperature, circulate 10 times like this, observe product deformation range whether within the scope of 0.2-0.5%, if belong to this scope, qualified, otherwise be considered as defective.
(9) material soaks the test of lithium-ion electrolyte cracking
The product of injection moulding is immersed in 24H in lithium-ion electrolyte, then left at room temperature 24H, and so circulation 10 times, sees whether product exists cracking phenomena.Wherein lithium-ion electrolyte comprises organic solvent and ionogen composition.Organic solvent is carbonates, as NSC 11801; Ionogen is lithium salts, as lithium perchlorate.
Above to invention has been detailed description; its object is to allow the personage being familiar with this art can understand content of the present invention and be implemented; can not limit the scope of the invention with this; and the invention is not restricted to the embodiments described; the equivalence change that all spirit according to the present invention are done or modification, all should be encompassed within protection scope of the present invention.
Claims (8)
1. polyphenylether resin alloy material, is characterized in that, with parts by weight, described polyphenylether resin alloy material comprises following recipe ingredient:
Polyphenylene oxide resin 40-60 part;
Polystyrene resin 20-60 part;
Polyolefine 1-3 part;
Elastomerics 1-8 part;
Fire retardant 1-15 part;
Glass fibre 10-20 part;
Grafting body 1-15 part;
Functional agglomerate 3-8 part;
Oxidation inhibitor 0.2-0.5 part;
Wherein:
Described elastomerics is one or several the mixture in styrene-butadiene rubber(SBR), HSBR, ethylene propylene rubber, terpolymer EP rubber, polyacrylic rubber, Toughening Effect of Ethylene Copolymer Elastomer, polyisoprene elastomerics, 1,2-polybutadiene elastomer;
Described grafting body is with the mixture of one or several in described polyphenylene oxide resin, polyolefine, elastomerics for base material, and the grafts of described grafting body is one or several the mixture in diacetyl oxide, propionic anhydride, Succinic anhydried, MALEIC ANHYDRIDE, benzoyl oxide, Tetra hydro Phthalic anhydride;
In described functional agglomerate gross weight for 100%, described functional agglomerate comprises following recipe ingredient:
At least one 70-90% in polyphenylene oxide resin, polystyrene resin, polyolefine or elastomerics;
Chirality mesoporous electro-conductive material 3-8%;
Lubricant 4-10%;
Chiral inorganic mesoporous material 3-15%;
Wherein:
Described chirality mesoporous electro-conductive material is at least one in polyaniline, polypyrrole;
Described lubricant is at least one in silicone oil, stearic acid lubricant;
Described chiral inorganic mesoporous material is at least one in silicon-dioxide, titanium dioxide.
2. polyphenylether resin alloy material according to claim 1, is characterized in that, described polyphenylene oxide resin is 2, the polymkeric substance of 6-xylenol, 2,6-xylenols and 2,3, the mixture of one or both in the multipolymer of 6-pseudocuminol, its limiting viscosity is 0.2-0.6dl/g.
3. polyphenylether resin alloy material according to claim 1, is characterized in that, described polystyrene resin is the mixture of the one or both in polystyrene, high-impact polystyrene.
4. polyphenylether resin alloy material according to claim 1, it is characterized in that, described polyolefine is one or several the mixture in polyethylene, polypropylene, ethylene propylene copolymer, polybutene, ethylene-butylene copolymer, ethene-unsaturated ester multipolymer.
5. according to the polyphenylether resin alloy material described in claim 1, it is characterized in that, described fire retardant is phosphorus flame retardant and nitrogen based flame retardant is the compound system that 2 ~ 4:1 forms by weight, wherein, described phosphorus flame retardant is the mixture of one or more in phosphate ester flame retardants, ammonium polyphosphate based flame retardant, inorganic phosphorus based flame retardant; Described nitrogen based flame retardant is melamine flame retardants.
6. according to the polyphenylether resin alloy material described in claim 1, it is characterized in that, described oxidation inhibitor is primary antioxidant and auxiliary antioxidant is the mixture that 1 ~ 3:1 forms by weight, wherein, described primary antioxidant is 3,5-di-t-butyl-4-hydroxy-phenylpropionic acid octadecyl, β-(3,5-di-t-butyl-4-hydroxy phenyl) propionic acid octadecyl, 2, one or several the mixture in 2 methylene-biss (4-methyl-6-tert-butylphenol); Described auxiliary antioxidant is one or several the mixture in three (Isosorbide-5-Nitrae-di-tert-butyl-phenyl) phosphorous acid, two (2,4-di-tert-butyl-phenyl) pentaerythritol diphosphate, two (octadecyl) pentaerythritol diphosphate.
7. a preparation method for the polyphenylether resin alloy material any one of claim 1 to 6 as described in claim, is characterized in that, described preparation method comprises the following steps:
(1) prepare functional agglomerate: by the formula of described functional agglomerate, utilize twin screw extruder extruding pelletization, temperature controls to melt extrude under 260-300 DEG C of condition, and main frame revolution controls at 250-350RPM, and vacuum degree control is at 0.5-0.8MPa;
(2) polyphenylether resin alloy material is prepared: by the formula of described polyphenylether resin alloy material, first described polyolefine, elastomerics, fire retardant, grafting body, functional agglomerate, oxidation inhibitor are mixed formation mixture, then, after described polyphenylene oxide resin, described polystyrene resin, described mixture and described glass fibre being added from the different charging openings of twin screw extruder, melt extrude.
8. the application of the polyphenylether resin alloy material as described in any one of claim 1 to 6 in lithium ion battery of electric automobile shell.
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| CN109852032A (en) * | 2019-02-13 | 2019-06-07 | 湖南恒屹新材料有限公司 | A kind of polyphenylene oxide resin based composites and its preparation method and application |
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| CN111560163A (en) * | 2020-05-24 | 2020-08-21 | 泗阳金拓驰环保科技有限公司 | PPO-PE-short glass fiber polymer alloy material and preparation method thereof |
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| CN101302336B (en) * | 2008-05-21 | 2011-03-16 | 深圳市科聚新材料有限公司 | Flame-retardant PPO/PA alloy and preparation thereof |
| CN102417718A (en) * | 2011-11-24 | 2012-04-18 | 上海日之升新技术发展有限公司 | Glass fiber reinforcement polyphenyl ether/polypropylene alloy and production method thereof |
| CN103122136A (en) * | 2013-02-05 | 2013-05-29 | 苏州市沃特新材料科技有限公司 | Polyphenylether composite material, and preparation method and application thereof |
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