CN1718635A - High toughness packing reinforced polyphenyl thioether composite material and its preparation method - Google Patents
High toughness packing reinforced polyphenyl thioether composite material and its preparation method Download PDFInfo
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Abstract
A high-toughness filler reinforced polyphenylthioether material with flame-retarding, thermal stable and mechanical performance is proportionally prepared from polyphenylthioether, glass fibres, inorganic mineral filler, impact modifier, coupling agent, antioxidizing agent and assistant.
Description
Technical field
The present invention relates to a kind of high toughness packing reinforced polyphenyl thioether composite material and preparation method thereof.
Background technology
Polyphenylene sulfide (PPS) claims polyphenylene sulfide, poly-phenylene thioether again, and nineteen sixty-eight is by a kind of new special engineering plastics of U.S. Phillips Petroleum Co. initiative and operation.Owing to have thiophenyl on its molecular backbone chain, the structure of sulphur atom and the mutual proper alignment of phenyl ring, give numberator height stable chemical bond characteristic, and be easy to be piled into the higher crystal lattice structure of thermostability, make it have many particular performances, mainly show: but the physical and mechanical property of good thermostability, chemical stability, dimensional stability, erosion resistance and electrical property excellence, good adhesiveproperties, good flame retardant resistance, good electrical properties blending and modifying.Have widely at aspects such as automobile making, electric, chemical industry, instrument and space industries at present and use.
Owing to the existence of phenyl ring a large amount of on the PPS main chain, increased the rigidity of material, make that unmodified polyphenyl thioether material fragility is bigger, mechanical property is poor, and heat resisting temperature is relatively low, has only 110 ℃, thereby the application of material is greatly limited.But, adopt glass fibre or inorganic mineral stopping composition to come modified polyphenyl thioether can improve its mechanical property and thermotolerance, heat-drawn wire can reach 260 ℃.But improve not quite for the impelling strength aspect that improves material, improve its impact property in order to enlarge its range of application, to press for.
Chinese patent CN1462771 adopts nanometer butadiene-styrene-vinyl rubber to come modified polyphenyl thioether, and this patent is mainly used in pure glass and strengthens polyphenylene sulfide, is not suitable for inorganic mineral and strengthens the filling polyphenyl thioether composite material.Same Chinese patent CN1513914 has proposed the employing olefine kind resin and polyphenylene sulfide forms a kind of polyphenylene sulfide composition, and this patent is not suitable for equally makes high enhancing polyphenyl thioether composite material of filling.
Continuous expansion along with the purposes of polyphenyl thioether material, high enhancing polyphenyl thioether material of filling content is used also extensive gradually, requirement to material is strict more, the resin composite materials that is proposed before this be can be described as insufficient, therefore require to develop and to satisfy higher forming process, shock-resistance, matrix material that cost is cheaper simultaneously.
Summary of the invention
The objective of the invention is to overcome the shortcoming that existing polyphenyl thioether composite material exists, a kind of both had high rigidity, corrosion-resistant, low creep are provided, have the polyphenyl thioether composite material of high impact toughness again.
Another object of the present invention provides the preparation method of above-mentioned polyphenyl thioether composite material.
In order to realize above purpose, technical scheme of the present invention provides a kind of high toughness packing reinforced polyphenyl thioether composite material, it is characterized in that forming: polyphenylene sulfide 25～65%, glass fibre 20～50%, inorganic mineral filler 0～40%, impact modifying agent 3～10%, coupling agent 0.2～1%, oxidation inhibitor 0.2～0.5%, processing aid 0.5～2% by following components in weight percentage.
Above-mentioned inorganic mineral filler is: one or more mixtures in talcum powder, lime carbonate, barium sulfate, calcium sulfate, wollastonite, kaolin, the glass microballon.The particle size range of inorganic mineral filler is 5～10 μ m.
Above-mentioned impact modifying agent is the blend of Hydrogenated SBS or styrene-acrylonitrile copolymer acid butyl ester binary graft modification ethylene-propylene rubber(EPR) (EPDM-g-St) and ethylene-methyl methacrylate Racemic glycidol fat.The adding of the impact modifying agent in the high toughness packing reinforced polyphenyl thioether composite material of the present invention mainly is to prevent that the adding of inorganic mineral filler from making material mechanical performance descend.The selection of impact modifying agent must consider that itself and resin should have good consistency, and impact modifying agent will form suitable phase structure and could more effectively improve toughening effect in material matrix simultaneously.
Above-mentioned oxidation inhibitor is one or more the mixture in phenolic antioxidant, phosphite ester kind antioxidant, the metal passivator.The purpose that adds oxidation inhibitor is for the thermostability that improves polyphenyl thioether composite material and further keeps high heat resistance.It is preferred 1010 wherein to be suitable for the phenolic antioxidant of body series, and phosphorous acid esters have TNP, 168, and metal passivator has GI-09-367, MD1025, OABH.Because phosphorous acid esters can be eliminated equally by ultraviolet ray and produce the peroxidation group, thereby also play the effect that prevents photoaging.
Above-mentioned coupling agent is one or more the mixture in silane coupling agent, titanate coupling agent, the aluminate coupling agent.As KH550, KH560, KH570, A-143, A-186, sulfonyl azide silane, NDZ-101, OL-1618 or the like.Coupling agent has improved the consistency between glass, inorganic mineral filler and resin, the plasticized modifier, strengthens the bounding force at interface between them, improves the mechanical property of material.
Above-mentioned processing aid is one or more the mixture in lipid acid, calcium stearate, Zinic stearas, silicone powder, the silicone master batch.The effect of processing aid is: add the dispersiveness that can effectively improve each component man-hour, reduce plastic melt and the bonding strength of metallic surface and the internal friction of plastic melt, product surface luster is poor when helping solving injection moulding, problems such as demoulding difficulty.
The preparation method of above-mentioned high toughness packing reinforced polyphenyl thioether composite material, for: with polyphenylene sulfide, inorganic mineral filler, glass fibre, impact modifying agent, coupling agent, oxidation inhibitor and processing aid in proportion after the high-speed mixer dispersing and mixing, by the twin screw extruder fusion, mixing, extrude, cool off, dry, pelletizing and packing.Each subregion temperature of used double-screw extruding machine barrel should remain between 240 ℃～310 ℃, and the length-to-diameter ratio of the screwing element of twin screw extruder is 30～40, and screw speed is 300～500 rev/mins.
Beneficial effect of the present invention: strengthen the polyphenylene sulfide mixture with traditional glass and compare, high toughness packing reinforced polyphenyl thioether composite material of the present invention had both improved toughness, had reduced the shrinking percentage of material, had improved mechanical performance of products again.That the high toughness packing reinforced polyphenyl thioether composite material of gained has is fire-retardant, environmental protection, thermally-stabilised, a series of outstanding advantages such as mechanical property good, easy machine-shaping, and Application Areas is very wide, comprises electric, electronic component, auto parts or the like field.
Embodiment
Embodiment 1～10
With polyphenylene sulfide, inorganic mineral filler, glass fibre, impact modifying agent, coupling agent, oxidation inhibitor and processing aid in proportion after the high-speed mixer dispersing and mixing, by the twin screw extruder fusion, mixing, extrude, cool off, dry, pelletizing and packing.Each subregion temperature of used double-screw extruding machine barrel should remain on 300 ℃, and the length-to-diameter ratio of the screwing element of twin screw extruder is 35, and screw speed is 400 rev/mins.
Prepare matrix material of the present invention according to last noodle producing method, embodiment 1～4 each component concentration such as table 1, embodiment 5～7 each component concentration such as tables 2, embodiment 8～10 each component concentration such as tables 3.The prepared mixture of each embodiment is injection molded into the standard batten of testing usefulness by standard size, and the physicals among each embodiment is tested by international standard respectively.Embodiment 1～4 has verified the consumption of different fillers, and other component is done corresponding the variation, and detailed data the results are shown in Table 1.Embodiment 5～7 has verified the consumption of impact modifying agent, and other component is done corresponding the variation, and detailed data the results are shown in Table 2.Embodiment 8～10 has verified that different fillers mix the rerum natura of using, and other component is done corresponding the variation, and detailed data the results are shown in Table 3.
Table 1, Example formulations table and composite properties detected result
| Component | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | |
| Polyphenylene sulfide | 63.5 | 53.5 | 43.5 | 33.5 | |
| Mineral filler | Lime carbonate | 10 | 20 | 30 | |
| Glass fibre | 30 | 30 | 30 | 30 | |
| Impact modifying agent | SEBS ethylene-methyl methacrylate Racemic glycidol fat | 2 3 | 2 3 | 2 3 | 2 3 |
| Coupling agent | KH560 | 0.5 | 0.5 | 0.5 | 0.5 |
| Oxidation inhibitor | 1010 168 | 0.2 0.3 | 0.2 0.3 | 0.2 0.3 | 0.2 0.3 |
| Processing aid | Silicone powder Zinic stearas | 0.25 0.25 | 0.25 0.25 | 0.25 0.25 | 0.25 0.25 |
| Physicals | |||||
| The Izod notched Izod impact strength | 11.2 | 10.5 | 9.6 | 9 | |
| Tensile strength | 142.5 | 141.3 | 147.6 | 148.9 | |
| Flexural strength | 190 | 199.6 | 208.3 | 209.8 | |
| Modulus in flexure | 10129 | 10250 | 12356 | 14631 | |
| Heat-drawn wire | 250 | 255 | 256 | 258 | |
| Density | 1.51 | 1.56 | 1.70 | 1.89 | |
Table 2, Example formulations table and composite properties detected result
| Component | Embodiment 5 | Embodiment 6 | Embodiment 7 | |
| Polyphenylene sulfide | 45.5 | 42.5 | 39.5 | |
| Mineral filler | Barium sulfate | 20 | 20 | 20 |
| Glass fibre | 30 | 30 | 30 | |
| Impact modifying agent | EPDM-g-St ethylene-methyl methacrylate Racemic glycidol fat | 1 2 | 2 4 | 3 6 |
| Coupling agent | KH550 | 0.5 | 0.5 | 0.5 |
| Oxidation inhibitor | 1010 TNP | 0.2 0.3 | 0.2 0.3 | 0.2 0.3 |
| Processing aid | The stearic acid calcium stearate | 0.25 0.25 | 0.25 0.25 | 0.25 0.25 |
| Physicals | ||||
| The Izod notched Izod impact strength | 7.8 | 9.5 | 11.5 | |
| Tensile strength | 147.3 | 137.6 | 125.9 | |
| Flexural strength | 189.6 | 178.3 | 168.8 | |
| Modulus in flexure | 12250 | 11436 | 9731 | |
| Heat-drawn wire | 260 | 256 | 250 | |
| Density | 1.70 | 1.69 | 1.68 | |
Table 3, Example formulations table and composite properties detected result
| Component | Embodiment 8 | Embodiment 9 | Embodiment 10 | |
| Polyphenylene sulfide | 35.5 | 35.5 | 35.5 | |
| Mineral filler | Talcum powder lime carbonate barium sulfate | 10 10 | 10 10 | 10 10 |
| Glass fibre | 40 | 40 | 40 | |
| Impact modifying agent | EPDM-g-St ethylene-methyl methacrylate Racemic glycidol fat | 1 2 | 1 2 | 1 2 |
| Coupling agent | KH550 | 0.5 | 0.5 | 0.5 |
| Oxidation inhibitor | 1010 TNP | 0.2 0.3 | 0.2 0.3 | 0.2 0.3 |
| Processing aid | The stearic acid calcium stearate | 0.25 0.25 | 0.25 0.25 | 0.25 0.25 |
| Physicals | ||||
| The Izod notched Izod impact strength | 8.4 | 10.8 | 8.5 | |
| Tensile strength | 135.5 | 148.3 | 147.8 | |
| Flexural strength | 186.5 | 205.6 | 218.3 | |
| Modulus in flexure | 16843 | 17850 | 18436 | |
| Heat-drawn wire | 265 | 260 | 260 | |
| Density | 1.89 | 1.90 | 1.89 | |
Claims (10)
1, a kind of high toughness packing reinforced polyphenyl thioether composite material, percentage ratio meter by weight, form by following component: polyphenylene sulfide 25～65%, glass fibre 20～50%, inorganic mineral filler 0～40%, impact modifying agent 3～10%, coupling agent 0.2～1%, oxidation inhibitor 0.2～0.5%, processing aid 0.5～2%.
2, high toughness packing reinforced polyphenyl thioether composite material according to claim 1 is characterized in that described inorganic mineral filler is: one or more mixtures in talcum powder, lime carbonate, barium sulfate, calcium sulfate, wollastonite, kaolin, the glass microballon.
3, high toughness packing reinforced polyphenyl thioether composite material according to claim 1 is characterized in that described impact modifying agent is the blend of Hydrogenated SBS or styrene-acrylonitrile copolymer acid butyl ester binary graft modification ethylene-propylene rubber(EPR) and ethylene-methyl methacrylate Racemic glycidol fat.
4, high toughness packing reinforced polyphenyl thioether composite material according to claim 1 is characterized in that described oxidation inhibitor is one or more the mixture in phenols, phosphorous acid esters, the metal passivator.
5, high toughness packing reinforced polyphenyl thioether composite material according to claim 4 is characterized in that described phenols is 1010; Described phosphorous acid esters are TNP or 168; Described metal passivator is GI-09-367, MD1025 or OABH.
6, high toughness packing reinforced polyphenyl thioether composite material according to claim 1, wherein said coupling agent are one or more the mixture in silane coupling agent, titanate coupling agent, the aluminate coupling agent.
7, high toughness packing reinforced polyphenyl thioether composite material as claimed in claim 6 is characterized in that described coupling agent is one or more the mixture among KH550, KH560, KH570, A-143, A-186, sulfonyl azide silane, NDZ-101, the OL-1618.
8, high toughness packing reinforced polyphenyl thioether composite material according to claim 1 is characterized in that described processing aid is one or more the mixture in lipid acid, calcium stearate, Zinic stearas, silicone powder, the silicone master batch.
9, high toughness packing reinforced polyphenyl thioether composite material as claimed in claim 2, the particle size range that it is characterized in that described inorganic mineral filler are 5～10 μ m.
10, the preparation method of the described high toughness packing reinforced polyphenyl thioether composite material of a kind of claim 1, for: with polyphenylene sulfide, inorganic mineral filler, glass fibre, impact modifying agent, coupling agent, oxidation inhibitor, processing aid in proportion after the high-speed mixer dispersing and mixing, by the twin screw extruder fusion, mixing, extrude, cool off, dry, pelletizing and packing.
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Assignee: Tianjin Kingfa New Materials Co., Ltd. Assignor: Golden hair Polytron Technologies Inc|Shanghai golden hair science and Technology Development Co., Ltd. Contract record no.: 2011440000009 Denomination of invention: High toughness packing reinforced polyphenyl thioether composite material and its preparation method Granted publication date: 20070509 License type: Exclusive License Open date: 20060111 Record date: 20110104 |