CN1737042A - Polyolefin composition and its preparation method and uses - Google Patents
Polyolefin composition and its preparation method and uses Download PDFInfo
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- CN1737042A CN1737042A CN 200410053834 CN200410053834A CN1737042A CN 1737042 A CN1737042 A CN 1737042A CN 200410053834 CN200410053834 CN 200410053834 CN 200410053834 A CN200410053834 A CN 200410053834A CN 1737042 A CN1737042 A CN 1737042A
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Abstract
The invention relates to a polyolefin composition and its preparation method and uses, wherein the constituents comprises (by weight ratio): thermoplastic elastomer 10-55%, mineral filler 35-85%, anti-oxidant 0.1-1%, surface processing agent 0.1-1%, processing auxiliary agent 3-15%. The produced polyolefin composition has good rigidity and tenacity, thus can be used for substituting PS (polystyrene) material in manufacturing outer casings or bases of various household electrical appliances.
Description
Technical field
The present invention relates to a kind of high-dimensional stability, high performance polyolefin compositions and its production and application.
Background technology
Polyethylene is a kind of half hitch crystal formation resin, and the dimensional contraction rate is big, and the shrinking percentage of polyvinyl resin is generally 1.6-2.2%, and dimensional stability is bad when being used to make big parts.Because poly rigidity and toughness are bad, are difficult to use in manufacturing and require to have favorable rigidity and flexible parts.The present invention obtains a kind of low-down dimensional stability that has, and has rigidity and flexible polyolefin compositions concurrently.Said composition can replace materials such as ABS, HIPS to be used to make parts such as televisor surgery, base plate of air conditioner.
By in the plastic working process, filler, toner, fire retardant, functional aid etc. being distributed to the carrier that has consistency with parent resin, can preparing the filler parent granule of the filler that contains high density, toner, fire retardant, functional aid.Filler parent granule has good dispersity, stable performance, and advantage such as easy to process is applied to the modification of polymkeric substance always.The filler parent granule of mineral filler adds in the polyolefin resin can bring bigger variation to performance.The present invention finds, by special production technique and prescription, can obtain a kind of rigidity and flexible filler parent granule that improves polyolefin resin simultaneously, and obtain a kind of low density, low-shrinkage, high rigidity and flexible polyolefin compositions of having concurrently.
Wang Yingjia has reported a kind of have excellent dispersiveness and mobile filling master batch in Chinese invention patent " parent material for filling of high-pressure polyethylene " (publication number 87107742.6).This master batch is made up of high-pressure polyethylene, activated calcium carbonate, adipocere.This filler parent granule does not possess the characteristics that high rigidity and high tenacity are provided.
Xu Shengxiu has reported a kind of plastic filler parent granule of high dispersive type in Chinese invention patent " plastic filler parent granule " (publication number 87102663).This filler parent granule as matrix, through auxiliary agent surface treatments such as chelating type phthalates, and is a carrier with petroleum resin, ethylene-propylene rubber(EPR), low-molecular-weight resin, dispersion agent, waste and old recovery polyolefin blend body by lime carbonate, forms through mixing, in blocks, pelletizing.This filler parent granule can not only not reduce the physical and mechanical properties of former plastics under bigger loading level, and its processing characteristics and physical and mechanical properties are increased substantially, so both reduced the plastics cost, improves its quality again.This filler parent granule does not have the characteristics of high tenacity.
Sun Shaoxuan has reported all purpose plastics packing parent grain that a kind of thermoplastics uses and preparation method thereof in Chinese invention patent " all purpose plastics packing parent grain and preparation method thereof " (1061028).Easy to use by general purpose grade plastic master batch provided by the invention, the performance that can regulate plastics is improved its result of use, and reduces its cost greatly, is an important channel of improving plastic products quality at present.It is formed through the granulation of kneading by the carrier polyethylene that is 1000-6000 through micronizing to filler zeolite and white carbon black, the molecular weight of 1-20 μ and conditioning agent turps and white oil or oneself penta tetrol methyl esters.The characteristics that do not possess high rigidity, high tenacity of this master batch.
Yan Yiliang, Yan Jinchun, Xie Mingjie are in Chinese invention patent " polyolefin modified filler parent granule and manufacture method thereof " (grant number CN 6107768B), reported a kind of, replaced the filler parent granule of traditional Atactic Polypropelene with rosin or rosin derivative coating agent as inorganic fillings.It is by following proportioning, makes through mixing, pelletizing.Its weight consists of: polyolefin resin 0-10%, and rosin or rosin derivative 0.3-15%, inorganic fillings 70-95% is applicable to the processing of various thermoplastic resins.Gained plastics performance has surpassed the requirement of the polyolefin master batch made from Atactic Polypropelene, and cheap, sufficient raw.But this filler parent granule does not obtain low density, low-shrinkage and toughness.
Ou Yuchun, Fang Xiaoping etc. have reported a kind of stuffing mother particle for toughening polyolefine and its production and use in Chinese invention patent " a kind of preparation method of stuffing mother particle for toughening polyolefine ".This filler parent granule comprises that particle dia is the mineral filler of 0.5 μ m-40 μ m, surface treatment agent, functionalization thermoplastic elastomer, thermoplastic resin and composition thereof, processing aid, behind above-mentioned each component uniform mixing, through twin screw extruder extrude or double roll mill mixing, granulation forms.Stuffing mother particle for toughening polyolefine of the present invention has mineral filler homodisperse in the master batch carrier, and with the polyolefine material compound tense, can be that the nuclear carrier is that " nuclear-shell " structured particles form of shell is distributed in the characteristics in the polyolefin substrate again with the mineral filler, its matrix material have reached high rigidity, high tenacity.In this patent and this filler parent granule of not mentioned application after can obtain to have high dimensional stability polyolefin compositions.
Ah portion wins; Ocean one is closed in the river; Star is wild real; The critical point restrains and reported a kind of method of making polyolefine resin composition the sixth of the twelve Earthly Branches in Chinese patent " a kind of stuffing mother particle for toughening polyolefine and its production and use "; it is that mineral filler is carried out abrasive dust and surface treatment with surface treatment agent in dry type or half dry type pulverizer; the mineral filler that to handle mixes with a certain amount of polyolefin resin and with the mixture pelleting that generates then, and the granular mixture that will obtain is thus expected with other or the pill polyolefin resin mixes with certain making a gesture of measuring again.This polyolefin compositions does not use filler parent granule, and the polyolefin compositions that obtains does not possess low-shrinkage.
Summary of the invention
The technical issues that need to address of the present invention are to disclose a kind of polyolefin compositions and its production and application, have the shortcoming of the polyolefin compositions of high rigidity, high tenacity, low density, high-dimensional stability concurrently with can not obtaining of overcoming that prior art exists.
The present invention also technical issues that need to address is to disclose a kind of thermoplastic elastomer filler parent granule.
The component and the weight percent content of thermoplastic elastomer filler parent granule of the present invention comprise:
Thermoplastic elastomer 10～55%
Mineral filler 35～85%
Oxidation inhibitor 0.1～1%
Surface treatment agent 0.1～1%
Processing aid 3～15%
Above-mentioned thermoplastic elastomer comprises styrene-butadiene rubber(SBR), paracril, cis-1,4-polybutadiene rubber, polyisoprene rubber, natural rubber, chloroprene rubber, ethene-alpha-olefin copolymer, ethylene-propylene-diene copolymer, ethylene-propylene rubber(EPR), ethylene-acrylic acid copolymer, ethylene-acrylate copolymer, ethylene-acrylate-glycidyl acrylate multipolymer, vinylbenzene-diene-styrene copolymer, vinyl-vinyl acetate copolymer, a kind of or its mixture in acrylate-styrene-butadiene copolymer;
Mineral filler comprises a kind of or its mixture in wollastonite, talcum powder, kaolin, polynite, mica, glass microballon, ceramic fine bead, glass microplate, titanium dioxide, magnesium hydroxide, the aluminium hydroxide;
Processing aid comprises that polyethylene wax, polyamide wax, polypropylene are cured, whiteruss, white oil, naphthenic oil, epoxy soybean oil or calcium stearate;
Surface treatment agent comprises a kind of or its mixture in γ～aminopropyltriethoxywerene werene, γ～propyl methacrylate base silane, γ～Racemic glycidol oxygen propyl trimethoxy silicane, γ～propylmercaptan Trimethoxy silane, positive titanium isopropylate, three (dioctylphyrophosphoric acid ester oxygen base) titanic acid ester, sec.-propyl three different stearoyl titanic acid ester, the stearic acid;
Oxidation inhibitor is selected from Hinered phenols antioxidant, phosphite ester kind antioxidant or contains a kind of or its mixture in the sulfur type antioxidant.
The component and the weight percent content of the polyolefin compositions that reaches of the present invention comprise:
Polyolefin resin 20～70%
Thermoplastic elastomer filler parent granule 5～50%
Mineral filler 5～40%
Functional polyolefin resin 2-25%
Coupling agent 0～0.5%
Oxidation inhibitor 0.1～1%
Above-mentioned polyolefin resin comprises a kind of or its mixture in high density polyethylene(HDPE), new LDPE (film grade), the medium-density polyethylene;
Functional polyolefin comprises a kind of or its mixture in maleic anhydride inoculated polypropylene, maleic anhydride grafted polyethylene, glycidyl acrylate graft polypropylene, glycidyl acrylate grafted polyethylene, the ethylene-acrylic acid glycidyl ester copolymer;
Mineral filler comprises a kind of or its mixture in wollastonite, chopped glass fiber, continuous glass-fiber, talcum powder, calcium carbonate crystal whisker, kaolin, polynite, mica, potassium titanate crystal whisker, glass microballon, ceramic fine bead, glass microplate, titanium dioxide, magnesium hydroxide, the aluminium hydroxide;
Coupling agent is selected from a kind of or its mixture in γ～aminopropyltriethoxywerene werene, γ～propyl methacrylate base silane, γ～Racemic glycidol oxygen propyl trimethoxy silicane, γ～propylmercaptan Trimethoxy silane, positive titanium isopropylate, three (dioctylphyrophosphoric acid ester oxygen base) titanic acid ester, the sec.-propyl three different stearoyl titanic acid ester;
Above-mentioned oxidation inhibitor comprises Hinered phenols antioxidant, phosphite ester kind antioxidant, contains a kind of or its mixture in the sulfur type antioxidant, as anti-oxidant Irganox 1010 (four [β-(3,5-di-t-butyl-4 hydroxy phenyl) propionic acid] defend the tetrol ester season), oxidation inhibitor Irgafos 168 3 ((2, the 4-di-tert-butyl-phenyl) phosphorous acid ester)
The preparation method of polyolefin compositions of the present invention comprises the steps:
With polyolefin resin, thermoplastic elastomer filler parent granule, mineral filler, functional polyolefin resin, coupling agent and oxidation inhibitor after the high mixer high speed mixes, melt extrude through two (list) screw extrusion presss, carry out granulation through tablets press again, can obtain said composition;
Wherein: the preparation method of said thermoplastic elastomer filler parent granule comprises the steps:
(1) thermoplastic elastomer was mixed 1～10 minute in the high mixer high speed with processing aid, mixing temperature is 25～70 ℃;
(2) with the product of step (1) and mineral filler, oxidation inhibitor, surface treatment agent high-speed mixer and mixing 1～35 minute, mixing temperature is 25～70 ℃, obtains blend;
(3) with blend under 160～220 ℃ through the twin screw extruder extruding pelletization.
Adopt the prepared polyolefin compositions of method of the present invention to have favorable rigidity and toughness simultaneously, can substituting PS (polystyrene) material, be mainly used in various appliance shells of preparation or base, such as televisor, air-conditioning washing machine shell, air-conditioning and washing machine pedestal, small household appliances shell and base etc.; Be used for IT product, such as computer housing and display casing, keyboard, mouse parts etc.; Be used for automotive upholstery, such as parts such as fascia, top board, internal hilar plate, handrails.
Embodiment
Adopt following material among the following embodiment:
The KH-550 (γ-An Jibingjisanyiyangjiguiwan) that Nanjing Shuguang Chemical General Plant produces
The anti-oxidant Irganox 1010 that Switzerland vapour Ba Jinghua company produces
The oxidation inhibitor Irgafox 168 that Switzerland vapour Ba Jinghua company produces
The EPDM ethylene-propylene-diene terpolymer that Ji Hua company produces
The TAMFER DF610 ethene-alpha-olefin copolymer that Mitsui produces
The polythene PE 5070 of Panjin petrochemical iy produced, and melt flow rate 7g/10min (190 ℃, 2.16kg)
Talcum powder, glass fibre, glass microballon, epoxy soybean oil, naphthenic oil, white oil, stearic acid are commercial chemical.
Embodiment 1-4
With 350g EPDM (vinylbenzene-diene-styrene copolymer), the 50g naphthenic oil adds in the high mixer, high mixing 3 minutes under normal temperature, drop into 1g anti-oxidant Irganox 1010 afterwards, 2g oxidation inhibitor Irgafos168,4g stearic acid, the 600g talcum powder continues high-speed mixing 15min.The Preblend that obtains obtains filler parent granule after twin screw extruder is extruded, each section extrusion temperature is set at 160 ℃-170 ℃-180 ℃-190 ℃-190 ℃-190 ℃-200 ℃.
Component and proportioning weighing material by table 1 provides mix in high-speed mixer, obtain composition after twin screw extruder is extruded.Each section extrusion temperature is set at 180 ℃-190 ℃-200 ℃-200 ℃-200 ℃-200 ℃-210 ℃.
The component of table 1 embodiment 1-4 and proportioning (following examples all by weight percentage)
| Component | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 |
| PE (polyethylene) thermoplastic elastomer (TPE) filler parent granule glass PE-g-MAH (maleic anhydride grafted polyethylene) KH-550 Irganox 1010 Irgafox 168 | 70 14.3 15 5 0.4 0.1 0.2 | 45 29.3 20 5 0.4 0.1 0.2 | 64.3 20 15 0.4 0.1 0.2 | 45 20 25 9.3 0.4 0.1 0.2 |
The performance (ASTM) of table 2 embodiment 1-4
| Test event | Unit | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 |
| The vertical shrinking percentage lateral shrinkage of tensile strength Izod notched Izod impact strength modulus in flexure density | MPa KJ/m 2 MPa g/cm 3 ％ ％ | 41 13 3540 1.15 0.4 0.5 | 40 22 3230 1.17 0.3 0.4 | 24 18 2620 1.14 0.4 0.5 | 47 19 5120 1.19 0.3 0.3 |
Embodiment 5-8 (Comparative Examples)
Component and proportioning weighing material by table 3 provides mix in high-speed mixer, obtain composition after twin screw extruder is extruded.Each section extrusion temperature is set at 190 ℃-200 ℃-200 ℃-200 ℃-200 ℃-210 ℃-210 ℃.
The component of table 3 embodiment 5-8 and proportioning (following examples all by weight percentage)
| Component | Embodiment 5 | Embodiment 6 | Embodiment 7 | Embodiment 8 |
| PP (polypropylene) EPDM (styrene-diene-styrene copolymer) talcum powder glass PP-g-MAH (maleic anhydride inoculated polypropylene) KH-550 Irganox 1010 Irgafox 168 | 70 7 12.3 5 5 0.4 0.1 0.2 | 54.3 10 20 15 5 0.4 0.1 0.2 | 64.3 7 13 15 0.4 0.1 0.2 | 44.3 7 13 25 5 0.4 0.1 0.2 |
The performance (ASTM) of table 4 embodiment 5-8
| Test event | Unit | Embodiment 5 | Embodiment 6 | Embodiment 7 | Embodiment 8 |
| The vertical shrinking percentage lateral shrinkage of tensile strength Izod notched Izod impact strength modulus in flexure density | MPa KJ/m 2 MPa g/cm 3 ％ ％ | 35 8 2015 1.15 0.6 1.1 | 36 9 2190 1.17 0.5 0.8 | 24 7 1960 1.14 0.5 0.9 | 40 8 3280 1.19 0.6 1.0 |
Claims (10)
1. a polyolefin compositions is characterized in that, component and weight percent content comprise:
Polyolefin resin 20～70%
Thermoplastic elastomer filler parent granule 5～50%
Mineral filler 5～40%
Functional polyolefin resin 2-25%
Coupling agent 0～0.5%
Oxidation inhibitor 0.1～1%.
2. polyolefin compositions according to claim 1 is characterized in that, polyolefin resin comprises a kind of or its mixture in high density polyethylene(HDPE), new LDPE (film grade), the medium-density polyethylene.
3. polyolefin compositions according to claim 1, it is characterized in that functional polyolefin comprises a kind of or its mixture in maleic anhydride inoculated polypropylene, maleic anhydride grafted polyethylene, glycidyl acrylate graft polypropylene, glycidyl acrylate grafted polyethylene, the ethene-glycidyl acrylate multipolymer.
4. polyolefin compositions according to claim 1, it is characterized in that mineral filler comprises a kind of or its mixture in wollastonite, chopped glass fiber, continuous glass-fiber, talcum powder, calcium carbonate crystal whisker, kaolin, polynite, mica, potassium titanate crystal whisker, glass microballon, ceramic fine bead, glass microplate, titanium dioxide, magnesium hydroxide, the aluminium hydroxide.
5. polyolefin compositions according to claim 1, it is characterized in that coupling agent is selected from a kind of or its mixture in γ～aminopropyltriethoxywerene werene, γ～propyl methacrylate base silane, γ～Racemic glycidol oxygen propyl trimethoxy silicane, γ～propylmercaptan Trimethoxy silane, positive titanium isopropylate, three (dioctylphyrophosphoric acid ester oxygen base) titanic acid ester, the sec.-propyl three different stearoyl titanic acid ester.
6. polyolefin compositions according to claim 1 is characterized in that, oxidation inhibitor comprises Hinered phenols antioxidant, phosphite ester kind antioxidant, contains a kind of or its mixture in the sulfur type antioxidant.
7. polyolefin compositions according to claim 1 is characterized in that, the component and the weight percent content of thermoplastic elastomer filler parent granule comprise:
Thermoplastic elastomer 10～55%
Mineral filler 35～85%
Oxidation inhibitor 0.1～1%
Surface treatment agent 0.1～1%
Processing aid 3～15%
Above-mentioned thermoplastic elastomer comprises styrene-butadiene rubber(SBR), paracril, cis-1,4-polybutadiene rubber, polyisoprene rubber, natural rubber, chloroprene rubber, ethene-alpha-olefin copolymer, ethene-propylene-diene copolymers, ethylene-propylene rubber(EPR), ethene-acrylic copolymer, ethene-acrylate copolymer, ethene-acrylate-glycidyl acrylate multipolymer, vinylbenzene-diene-styrol copolymer, the ethylene-vinyl acetate ester copolymer, a kind of or its mixture in acrylate-vinylbenzene-butadienecopolymer;
Mineral filler comprises a kind of or its mixture in wollastonite, talcum powder, kaolin, polynite, mica, glass microballon, ceramic fine bead, glass microplate, titanium dioxide, magnesium hydroxide, the aluminium hydroxide;
Processing aid comprises that polyethylene wax, polyamide wax, polypropylene are cured, whiteruss, white oil, naphthenic oil, epoxy soybean oil or calcium stearate;
Surface treatment agent comprises a kind of or its mixture in γ～aminopropyltriethoxywerene werene, γ～propyl methacrylate base silane, γ～Racemic glycidol oxygen propyl trimethoxy silicane, γ～propylmercaptan Trimethoxy silane, positive titanium isopropylate, three (dioctylphyrophosphoric acid ester oxygen base) titanic acid ester, sec.-propyl three different stearoyl titanic acid ester, the stearic acid;
Oxidation inhibitor is selected from Hinered phenols antioxidant, phosphite ester kind antioxidant or contains a kind of or its mixture in the sulfur type antioxidant.
8. the preparation method according to each described polyolefin compositions of claim 1～7 comprises the steps:
With polyolefin resin, thermoplastic elastomer filler parent granule, mineral filler, functional polyolefin resin, coupling agent and oxidation inhibitor after the high mixer high speed mixes; melt extrude through two (list) screw extrusion presss; carry out granulation through tablets press again, can obtain said composition.
9. method according to claim 8 is characterized in that, said thermoplastic elastomer filler parent granule is preparation like this:
(1) thermoplastic elastomer was mixed 1～10 minute in the high mixer high speed with processing aid, mixing temperature is 25～70 ℃;
(2) with the product of step (1) and mineral filler, oxidation inhibitor, surface treatment agent high-speed mixer and mixing 1～35 minute, mixing temperature is 25～70 ℃, obtains blend;
(3) with blend under 160～220 ℃ through the twin screw extruder extruding pelletization.
10. the application of each described polyolefin compositions of claim 1～7 is characterized in that, is used to prepare appliance shell, base, IT product, cabinet, display casing, keyboard, mouse parts, automotive upholstery.
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| CN 200410053834 CN1737042A (en) | 2004-08-18 | 2004-08-18 | Polyolefin composition and its preparation method and uses |
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| CN104212046B (en) * | 2014-08-18 | 2018-02-09 | 陕西中昌科技有限公司 | Porous plum tube and preparation method thereof |
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