CN1112401C - Weather-resistant high-flowbility fireproof shock-resistant polystyrene composite with less environment pollution - Google Patents
Weather-resistant high-flowbility fireproof shock-resistant polystyrene composite with less environment pollution Download PDFInfo
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- CN1112401C CN1112401C CN 00124685 CN00124685A CN1112401C CN 1112401 C CN1112401 C CN 1112401C CN 00124685 CN00124685 CN 00124685 CN 00124685 A CN00124685 A CN 00124685A CN 1112401 C CN1112401 C CN 1112401C
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Abstract
The present invention provides a weathering resisting, flame retarding, high fluidity and high impact polystyrene composition conforming to the requirement for environmental protection and a preparation method thereof. The composition is prepared from 60 to 85 wt% of high impact polystyrene (HIPS for short in English) resin, 5 to 25 wt% of flame retardant, 1 to 6 wt% of flame retarding synergist, 2 to 20 wt% of impact modifier, 0.2 to 7 wt% of photostabilizer, 0.1 to 1 wt% of antioxidant, 0.2 to 1 wt% of coupler and 0.5 to 5 wt% of other processing aids according to certain mixture proportion through secondary extrusion processing via a double-screw extruding machine. The composition of the present invention has the advantages of high-grade flame retarding performance, little environmental pollution, little damage to human bodies, easy forming, good surface gloss, photoaging resistance, etc. The composition of the present invention conforms to the strict international requirement for environmental protection at present. The composition is suitable for the manufacture of outer shells of various household electric appliance products.
Description
The present invention relates to a kind of weather-resistant high-flowbility fireproof shock-resistant polystyrene composite with less environment pollution and preparation method thereof.
Polystyrene (PS) is to realize industrialization by German I.G method our company (predecessor of BASF AG) in nineteen thirty.As one of five big general-purpose plastics, it has, and formability is good, matter is hard, transparent, rigidity, electrical insulating property, agent of low hygroscopicity, dyeing and advantage such as cheap easily.Generate high-impact polystyrene (HIPS) mixes a small amount of elastomerics in PS after, it has overcome the crisp shortcoming of polystyrene, thereby is widely used in industries such as electronics, automobile, household electrical appliances, instrument, daily necessities, toy.But HIPS burns easily, and weathering resistance is poor, and mobile difference can not be fit to make shortcomings such as surface requirements height and large thin-wall goods after the modification, has limited it and has further promoted the use of.Particularly enter the very promising light household electric appliances field of tool at present such as indicating meter, video recorder, duplicating machine, facsimile recorder, printer, conditioner, refrigerator.(referring to PlasticsTechnology, 1995,41 (1): 36～40)
What occur at present much aiming at such use and the flame-retarding HIPS kind ubiquity some shortcomings developed.As adopt the fire-retardant polystyrene mechanical property of decabromodiphenyl oxide (being DBDPO), tetrabromo-bisphenol good, flame retarding efficiency height, but weathering resistance is poor, goods in use be subjected to ultraviolet influence easily and produce variable color, problem such as become fragile.And studies show that among the DBDPO in recent years exists and may limit use in several European countries to cancer De Er Evil Young/two furans problems.Therefore in fire-retardant development from now on, must consider the compatibility problem of material and environment.The Liu Sufang of Shanxi-Prov Inst of Chemical Industry has done row ground discussion (referring to plastics communication 95 (4) 25～28) in detail to this.
Adopt effectively flame-retarding HIPS of clorafin, do not have Er Evil Young/two furans problems simultaneously, but its poor stability, its decomposition temperature has only 170 ℃, is lower than the processing temperature of HIPS, and its degradation production hydrogenchloride has serious corrosive nature to mould simultaneously.(referring to EP509535)
Adopt the fire-retardant HIPS of phosphorus nitrogen systems not have Er Evil Young/two furans problems, but because loading level is big, poor with the consistency of resin matrix, can make the mechanical properties decrease of material very big, be not suitable for the occasion high to material performance requirement.(referring to plastics exploitation 2000 (26) 1287～1293)
Adopt the flame-retarding HIPS of ethyl-two (tetrabromo phthalimide) based flame retardants and photostabilizer paralled system to have good weathering resistance, do not have Er Evil Young/two furans problems.But because ethyl-two (tetrabromo phthalimide) based flame retardant fusing point height is mobile poor, be not suitable for the gas assisted molding technology that is used for injection moulding of large thin-wall goods and current trend, the surface luster of goods is poor simultaneously.(referring to JP0415248)
Problem at the current material appearance, the mobile flame-proof highly anti-flush polyphenylacetylene of the weather-proof height of environment-friendly type provided by the invention has kept the premium properties of HIPS resin, flame retardant rating reaches the UL94V-0 level, with the no Er Evil of good of Environmental compatibility Young/two furans problems, ultraviolet light and thermal ageing are strong, Heat stability is good, mobile high, product surface gloss.Has higher utility.
Fire retardant in the weather-resistant high-flowbility fireproof shock-resistant polystyrene composite with less environment pollution of the present invention is a composite flame-retardant agent, and main flame retardant is that ethyl-(molecular formula is C to two (many bromines phthalic imidine) compounds fire retardant
18H
4O
4N
2Br
n, wherein n is 4～8), bromination epoxy oligomer (BEO, molecular weight 720～50000, bromine content 46～54%), do not contain the mixture of the modification bromination epoxy oligomer (MBEO, molecular weight 1000～100000) of Polybrominated biphenyl structure.More than several based flame retardants very high thermostability (being higher than 350 ℃) is all arranged and does not contain Poly Brominated Diphenyl Ethers (DPO) structure.While ethyl-two (many bromines face Phthalimide) compounds fire retardant good weatherability, the flame retarding efficiency height; Bromination epoxy oligomer and modification bromination epoxy oligomer good weatherability, good fluidity.Therefore two based flame retardants are composite can obtain very good fire-retardant and processing effect.
Retardant synergist in the weather-resistant high-flowbility fireproof shock-resistant polystyrene composite with less environment pollution of the present invention has the mixture of antimonous oxide, stibnate, borate, metaborate, molybdenum oxide, tetrafluoroethylene, phosphorous acid esters and/or these compounds.Antimonous oxide, stibnate, borate, metaborate can improve the flame retarding efficiency of fire retardant, molybdenum oxide has the cigarette effect of pressing down, tetrafluoroethylene has the effect of the fusion of preventing drippage, and phosphorous acid esters (three (nonyl) phosphorous acid ester) have the effect that prevents surplus combustion when burning.Adopt multiple retardant synergist recombination energy to make flame retardant effect more remarkable.
The adding of the impact modifying agent in the weather-resistant high-flowbility fireproof shock-resistant polystyrene composite with less environment pollution of the present invention mainly is to prevent that the adding of fire retardant 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.The impact modifying agent that uses among the present invention is styrene isoprene styrene block copolymer (SIS) (SIS), styrene-butadiene-styrene block copolymer (SBS), Hydrogenated SBS, styrene-acrylonitrile copolymer acid butyl ester binary graft modification ethylene-propylene rubber(EPR) (EPDM-g-St) etc.
Photostabilizer in the weather-resistant high-flowbility fireproof shock-resistant polystyrene composite with less environment pollution of the present invention is benzophenone, dimethylbenzene ketone, benzotriazole category, hindered amines, titanium dioxide, zinc oxide etc.The complex light stabilising system of employing above-claimed cpd can be brought into play the light aging resisting effect of photostabilizer to greatest extent.As Tinuvin327/Tinuvin770/TiO
2The complex light stabilising system.These photostabilizers include UVO, UV9, UV531, Tinuvin327, Tinuvin770, Tinuvin120, Tinuvin744, GW540, Epu, R69.
Oxidation inhibitor in the weather-resistant high-flowbility fireproof shock-resistant polystyrene composite with less environment pollution of the present invention is phenols, phosphorous acid esters, contain the mixture of thioesters class, metal passivator and/or these compounds.The phenolic antioxidant that wherein is suitable for body series has 2,4, and 6-BHT, E-330,2246,1010, phosphorous acid esters have TNP, 168, and containing the thioesters class is DLTP, DSTP, 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.
Coupling agent in the weather-resistant high-flowbility fireproof shock-resistant polystyrene composite with less environment pollution of the present invention also can be used the mixture of silane coupling agent and/or titanate coupling agent, aluminate coupling agent for being silane coupling agent.As KH570, A-143, A-186, sulfonyl azide silane, NDZ-101, OL-1618.Coupling agent has improved the consistency between fire retardant and resin, the plasticized modifier, strengthens the bounding force at interface between them, improves the mechanical property of material.
Other processing aid in the weather-resistant high-flowbility fireproof shock-resistant polystyrene composite with less environment pollution of the present invention is fatty acid amide, fatty acid compound, paraffin, white mineral oil, silicone mixture etc.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, the weld mark that occurs in the product when helping solving injection moulding, surface luster is poor, problems such as demoulding difficulty
Its preparation method in the weather-resistant high-flowbility fireproof shock-resistant polystyrene composite with less environment pollution of the present invention is to adopt high speed pre-mixing and dispersing secondary expressing technique.With fire retardant, retardant synergist, impact modifying agent, coupling agent blend extruding pelletization, obtain fire-retardant toughened masterbatch 1 earlier.And then with fire-retardant toughened masterbatch 1 and high-impact polystyrene resin and other additive after dispersing and mixing, by the twin screw extruder fusion, mixing, extrude, cool off, dry, pelletizing and packing.The benefit of such secondary expressing technique is the fire-retardant toughened masterbatch 1 that obtains by the first step, and a spot of impact modifying agent just closely disperses fire retardant, retardant synergist to coat.Again when these masterbatch and high-impact polystyrene resin and other additive during through blending dispersion, because impact modifying agent and high-impact polystyrene resin have fine consistency, impact modifying agent forms one deck flexible between resin and fire retardant, in conjunction with firm interfacial layer, reduced the influence of fire retardant effectively to the resin mechanical property.This impact modifying agent makes flame-retardant system obtain well to disperse, and fire retardant has increased the effect of effective toughness reinforcing volume of impact modifying agent and improved flame retarding efficiency and toughening efficiency greatly.Compare with an expressing technique, fire retardant can reduce 10～20%, and impact modifying agent can be less with 20～60%.And the constant product quality of gained.
Compare with traditional flame-proof highly anti-flush polyphenylacetylene resin complexes, weather-resistant high-flowbility fireproof shock-resistant polystyrene composite with less environment pollution of the present invention has adopted novel flame retardant composites system, selected new impact modifying agent for use, optimized light, heat, oxygen aging stabilising system and processing aid system, the secondary that creates a kind of efficient stable is simultaneously extruded complete processing.That the weather-resistant high-flowbility fireproof shock-resistant polystyrene composite with less environment pollution of gained has is fire-retardant, environmental protection, weather-proof, thermally-stabilised, a series of outstanding advantages such as mechanical property is good, easy machine-shaping, is very suitable for the very promising light household electric appliances field of tool at present such as indicating meter, video recorder, duplicating machine, facsimile recorder, printer, conditioner, refrigerator.
The present invention is verified by following embodiment:
The preparation of weather-resistant high-flowbility fireproof shock-resistant polystyrene composite with less environment pollution of the present invention and physicals see Table 1 and 2.This test employing divinyl rubber content is 3～10% HIPS, and fire retardant ethyl-two (tetrabromo phthalimide) adopts U.S. Albemarle Corporation product, and the trade mark is BT-93.Flame retardant brominated epoxy oligomer (BEO) and the modification bromination epoxy oligomer (MBEO) that does not contain the Polybrominated biphenyl structure are the product of Israel Dead Sea bromine company.Impact modifying agent is styrene/acrylic butyl ester binary graft modification EPDM (EPDM-g-St/BA).
EPDM-g-St/BA can be by the formulation of table 1:
Table 1
Raw material ratio (weight)
EPDM 50
Hexanaphthene 935
Peroxide C HP 0.5
Styrene monomer 10
Butyl acrylate 5
Concrete preparation method is: earlier EPDM is dissolved in the cyclohexane solvent, is heated to 70～80 ℃ while stirring, constant temperature.Styrene monomer, butyl acrylate and peroxide C HP are mixed the back slowly add, constant temperature stirred 5～7 hours in 70～80 ℃ then.Adding flocculation agent precipitation, filtration, washing, drying are waited until product EPDM-g-St/BA.The gel fraction of modified product is 10～30%, percentage of grafting 20～50%, and transformation efficiency is greater than 95%.
Because partial cross-linked EPDM has very low second-order transition temperature, higher intensity.Styrene/acrylic butyl ester multipolymer in the grafting not only has good consistency with HIPS, and because the existence of butyl acrylate makes grafted chain have good kindliness.These characteristics make EPDM-g-St/BA that HIPS is had good toughening effect, can keep the rigidity of HIPS again.
The concrete operation steps of weather-resistant high-flowbility fireproof shock-resistant polystyrene composite with less environment pollution embodiment of the present invention is:
With plasticized modifier, fire retardant, retardant synergist, and coupling agent behind thorough mixing under the high-speed stirring, carry out granulation, fire-retardant toughened masterbatch 1 with twin screw extruder.Prilling temperature is 160 ℃～250 ℃.
With fire-retardant toughened masterbatch 1 and high-impact polystyrene resin and other additive after dispersing and mixing, by the twin screw extruder fusion, mixing, extrude, cool off, dry, pelletizing and packing.Each subregion temperature of barrel should remain between 180 ℃～260 ℃
The twin screw extruder length-to-diameter ratio that is applied to preparation method of the present invention is 32～40, and screw speed is 300～500 rev/mins.
The mixture of each embodiment preparation is injection molded into the standard batten of testing usefulness by standard size, and the physicals among each embodiment is respectively by China's national standard and U.S. UL standard testing, and is as shown in table 2:
Table 2
Physicals unit testing method
Melting index g/10min GB3682
Tensile strength MPa GB1040 elongation at break % GB1040Izod notched Izod impact strength KJ/m
2GB1843 heat-drawn wire ℃ GB1634 modulus in flexure MPa GB9341 flexural strength MPa GB9341 incendivity UL94 xenon lamp artificial accelerated aging performance
GB9344 (300hour) Izod notched Izod impact strength KJ/m
2GB1843 value of chromatism DE (300hour) GB250
Embodiment formula table and composite properties detected result see Table 3
Table 3 component 12345
*Resin HIPS 100 73.2 64.2 69.2 69.2
BT-93 12 333 fire retardant BEO (FR-2400) 17
MBEO(FR-3030) 12 12
The zinc borate 6777 fire-retardant tetrafluoroethylene 0.3 0.3 0.3 0.3 that increase are imitated agent three (nonyl) phosphorous acid
1 1 1 1
Ester impacts and changes
EPDM-g-St/BA 3333 property agent
Titanium dioxide 2222 weather resisting agent UV-327 0.2 0.2 0.2 0.2
UV-770 0.4 0.4 0.4 0.4 coupling agent sulfonyl azide silane 0.5 0.5 0.5 0.5
BHT 0.2 0.2 0.2 0.2 oxidation inhibitor
168 0.2 0.2 0.2 0.2
Stearylamide 0.5 0.5 0.5 0.5 processing help
0.25 0.25 0.25 0.25 dose of calcium stearate
Butyl stearate 0.25 0.25 0.25 0.25 physical property melt index 2.7 3.0 16 15 15 hot strengths 27 25 23 25 24 elongation at breaks 40 40 30 45 45Izod notched Izod impact strength 11 8 10 11 8 heat distortion temperatures 85 80 78 80 78 bending modulus 2,300 2,100 2,100 2,100 2100 bending strengths, 39 36 34 35 35 flammabilities (1.6mm) HB V-0 V-0 V-0 V-1 xenon lamp artificial accelerated aging performances
(300hour) the Izod notched Izod impact strength 46797
DE 25 0.9 1.1 1.8 1.8
*.2,3, No. 4 prescriptions adopt secondaries to extrude, and once extrude after No. 5 prescription adopts all raw material to mix, its shock strength and combustionproperty be the mixture not as extruding through secondary all.
Claims (6)
1, a kind of weather-resistant high-flowbility fireproof shock-resistant polystyrene composite with less environment pollution, its feature consists of: high-impact polystyrene resin 60～85 weight %, fire retardant 5～25 weight %, retardant synergist 1～6 weight %, impact modifying agent 2～20 weight %, photostabilizer 0.2～7 weight %, oxidation inhibitor 0.1～1 weight %, coupling agent 0.2～1 weight %, other processing aid 0.5～5 weight %, wherein said fire retardant are ethyl-two (many bromines phthalic imidine) compounds fire retardant and bromination epoxy oligomer or the mixture that does not contain the modification bromination epoxy oligomer of Polybrominated biphenyl structure; Described retardant synergist is the mixture of antimonous oxide, stibnate, borate, metaborate, molybdenum oxide, tetrafluoroethylene, phosphorous acid esters and/or these compounds; Described impact modifying agent is the mixture of styrene isoprene styrene block copolymer (SIS), styrene butadiene one styrene block copolymer, hydrogenated styrene-butadiene-styrene block copolymers, styrene-acrylonitrile copolymer acid butyl ester binary graft modification ethylene-propylene rubber(EPR) and/or these compounds.
2, weather-resistant high-flowbility fireproof shock-resistant polystyrene composite with less environment pollution according to claim 1, wherein photostabilizer is the mixture of benzophenone, dimethylbenzene ketone, benzotriazole category, hindered amines, titanium dioxide, zinc oxide, carbon black and/or these compounds.
3, weather-resistant high-flowbility fireproof shock-resistant polystyrene composite with less environment pollution according to claim 1, wherein oxidation inhibitor is phenols, phosphorous acid esters, contains the mixture of thioesters class, metal passivator and/or these compounds.
4, weather-resistant high-flowbility fireproof shock-resistant polystyrene composite with less environment pollution according to claim 1, wherein said coupling agent are the mixture of silane coupling agent, titanate coupling agent, aluminate coupling agent and/or these coupling agents.
5, weather-resistant high-flowbility fireproof shock-resistant polystyrene composite with less environment pollution according to claim 1, wherein said other processing aid are the mixture of fatty acid amide, fatty acid mixture, paraffin, white mineral oil, alpha-methyl styrene and/or these mixtures.
6, this method of method for preparing the described weather-resistant high-flowbility fireproof shock-resistant polystyrene composite with less environment pollution of claim 1 comprises earlier with fire retardant, retardant synergist, impact modifying agent, coupling agent elder generation blend extruding pelletization, obtain fire-retardant toughened masterbatch 1, and then with fire-retardant toughened masterbatch 1 and high-impact polystyrene resin and other additive after dispersing and mixing, by the twin screw extruder fusion, mixing, extrude, cool off, dry, pelletizing and packing.
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Cited By (1)
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| CN101372548B (en) * | 2008-10-15 | 2011-01-19 | 珠海市远康企业有限公司 | High-impact polystyrene blend and preparation thereof |
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| CN101486824B (en) * | 2008-01-17 | 2012-06-27 | 深圳市亚塑科技有限公司 | Preparation of low temperature resistant environment friendly flame-retardant high impact resistance polystyrene composition |
| CN101817959B (en) * | 2009-12-30 | 2012-10-03 | 上海锦湖日丽塑料有限公司 | Flame-retardant styrene resin composition for large-scale thin wall parts and preparation method thereof |
| CN102372896B (en) * | 2010-08-13 | 2013-09-18 | 上海锦湖日丽塑料有限公司 | Low-odor flame retardant styrene-based resin composition and preparation method thereof |
| CN102115571A (en) * | 2010-12-30 | 2011-07-06 | 佛山市顺德区圆融新材料有限公司 | Weather-resistant high impact polystyrene material and preparation method thereof |
| CN103146090A (en) * | 2011-12-07 | 2013-06-12 | 滁州格美特科技有限公司 | Weather-resistant, flame retardant and impact-resistant polystyrene material, and preparation method |
| CN105385006A (en) * | 2015-12-04 | 2016-03-09 | 简淦欢 | Impact-resistant polystyrene with high performance on resisting heat and oil product |
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| CN106188925A (en) * | 2016-08-09 | 2016-12-07 | 叶剑 | A kind of polyphenylacetylene combination for clad plate and manufacture method thereof |
| CN106751337A (en) * | 2016-12-14 | 2017-05-31 | 广东圆融新材料有限公司 | A kind of LED printing opacity display HIPS materials and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101372548B (en) * | 2008-10-15 | 2011-01-19 | 珠海市远康企业有限公司 | High-impact polystyrene blend and preparation thereof |
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