CN102827421A - Polypropylene material and preparation method thereof - Google Patents
Polypropylene material and preparation method thereof Download PDFInfo
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- CN102827421A CN102827421A CN2012103238262A CN201210323826A CN102827421A CN 102827421 A CN102827421 A CN 102827421A CN 2012103238262 A CN2012103238262 A CN 2012103238262A CN 201210323826 A CN201210323826 A CN 201210323826A CN 102827421 A CN102827421 A CN 102827421A
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- polypropylene material
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- hindered amine
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- -1 Polypropylene Polymers 0.000 title claims abstract description 108
- 239000000463 material Substances 0.000 title claims abstract description 87
- 239000004743 Polypropylene Substances 0.000 title claims abstract description 78
- 229920001155 polypropylene Polymers 0.000 title claims abstract description 67
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000000178 monomer Substances 0.000 claims abstract description 26
- 239000011347 resin Substances 0.000 claims abstract description 4
- 229920005989 resin Polymers 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims abstract 3
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 13
- 229920002554 vinyl polymer Polymers 0.000 claims description 13
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical group C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 claims description 12
- DAKWPKUUDNSNPN-UHFFFAOYSA-N Trimethylolpropane triacrylate Chemical group C=CC(=O)OCC(CC)(COC(=O)C=C)COC(=O)C=C DAKWPKUUDNSNPN-UHFFFAOYSA-N 0.000 claims description 7
- 229920000468 styrene butadiene styrene block copolymer Polymers 0.000 claims description 7
- FACXGONDLDSNOE-UHFFFAOYSA-N buta-1,3-diene;styrene Chemical compound C=CC=C.C=CC1=CC=CC=C1.C=CC1=CC=CC=C1 FACXGONDLDSNOE-UHFFFAOYSA-N 0.000 claims description 6
- 238000001125 extrusion Methods 0.000 claims description 6
- 238000005469 granulation Methods 0.000 claims description 6
- 230000003179 granulation Effects 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 5
- HVVWZTWDBSEWIH-UHFFFAOYSA-N [2-(hydroxymethyl)-3-prop-2-enoyloxy-2-(prop-2-enoyloxymethyl)propyl] prop-2-enoate Chemical compound C=CC(=O)OCC(CO)(COC(=O)C=C)COC(=O)C=C HVVWZTWDBSEWIH-UHFFFAOYSA-N 0.000 claims description 4
- 239000003963 antioxidant agent Substances 0.000 claims description 4
- 230000003078 antioxidant effect Effects 0.000 claims description 4
- 229920003048 styrene butadiene rubber Polymers 0.000 claims description 4
- KOMNUTZXSVSERR-UHFFFAOYSA-N 1,3,5-tris(prop-2-enyl)-1,3,5-triazinane-2,4,6-trione Chemical compound C=CCN1C(=O)N(CC=C)C(=O)N(CC=C)C1=O KOMNUTZXSVSERR-UHFFFAOYSA-N 0.000 claims description 3
- 229920000459 Nitrile rubber Polymers 0.000 claims description 3
- 239000002202 Polyethylene glycol Substances 0.000 claims description 3
- 125000004386 diacrylate group Chemical group 0.000 claims description 3
- 229920001223 polyethylene glycol Polymers 0.000 claims description 3
- 229920002725 thermoplastic elastomer Polymers 0.000 claims description 3
- 229920002943 EPDM rubber Polymers 0.000 claims description 2
- 239000012745 toughening agent Substances 0.000 claims 3
- 229920001577 copolymer Polymers 0.000 claims 2
- OQLRBFNNEQUJPK-UHFFFAOYSA-N (3,5-ditert-butyl-4-hydroxyphenyl)methyl diethyl phosphate Chemical group CCOP(=O)(OCC)OCC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 OQLRBFNNEQUJPK-UHFFFAOYSA-N 0.000 claims 1
- VSYDLUXFKAXBBY-UHFFFAOYSA-N C(C=1C(C(=O)O)=CC=CC1)(=O)O.C(C=C)(=O)O.C(C=C)(=O)O.C(COCCO)O Chemical compound C(C=1C(C(=O)O)=CC=CC1)(=O)O.C(C=C)(=O)O.C(C=C)(=O)O.C(COCCO)O VSYDLUXFKAXBBY-UHFFFAOYSA-N 0.000 claims 1
- 244000043261 Hevea brasiliensis Species 0.000 claims 1
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 claims 1
- 229920003052 natural elastomer Polymers 0.000 claims 1
- 229920001194 natural rubber Polymers 0.000 claims 1
- 238000012986 modification Methods 0.000 abstract description 10
- 230000004048 modification Effects 0.000 abstract description 10
- 125000003342 alkenyl group Chemical group 0.000 abstract description 3
- 229920002521 macromolecule Polymers 0.000 abstract description 2
- 239000004611 light stabiliser Substances 0.000 abstract 3
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 abstract 1
- 239000005977 Ethylene Substances 0.000 abstract 1
- 238000004132 cross linking Methods 0.000 abstract 1
- 230000001678 irradiating effect Effects 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 description 23
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 18
- 230000032683 aging Effects 0.000 description 16
- 239000000203 mixture Substances 0.000 description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
- 239000013067 intermediate product Substances 0.000 description 10
- 239000004594 Masterbatch (MB) Substances 0.000 description 9
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 9
- 125000003368 amide group Chemical group 0.000 description 9
- 238000000034 method Methods 0.000 description 9
- 150000001875 compounds Chemical class 0.000 description 8
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 8
- 239000003112 inhibitor Substances 0.000 description 8
- 239000003960 organic solvent Substances 0.000 description 8
- 238000005453 pelletization Methods 0.000 description 8
- 230000001681 protective effect Effects 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 230000005855 radiation Effects 0.000 description 7
- 239000012298 atmosphere Substances 0.000 description 6
- 230000000903 blocking effect Effects 0.000 description 6
- 229920001971 elastomer Polymers 0.000 description 6
- 230000014759 maintenance of location Effects 0.000 description 6
- 230000003647 oxidation Effects 0.000 description 6
- 238000007254 oxidation reaction Methods 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- GFLJTEHFZZNCTR-UHFFFAOYSA-N 3-prop-2-enoyloxypropyl prop-2-enoate Chemical compound C=CC(=O)OCCCOC(=O)C=C GFLJTEHFZZNCTR-UHFFFAOYSA-N 0.000 description 5
- 229920000178 Acrylic resin Polymers 0.000 description 5
- 239000004925 Acrylic resin Substances 0.000 description 5
- 239000012752 auxiliary agent Substances 0.000 description 5
- 239000003153 chemical reaction reagent Substances 0.000 description 5
- 238000001816 cooling Methods 0.000 description 5
- 238000010511 deprotection reaction Methods 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- 229920000371 poly(diallyldimethylammonium chloride) polymer Polymers 0.000 description 5
- 230000035939 shock Effects 0.000 description 5
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 4
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- 239000007864 aqueous solution Substances 0.000 description 4
- 239000011230 binding agent Substances 0.000 description 4
- MGNCLNQXLYJVJD-UHFFFAOYSA-N cyanuric chloride Chemical compound ClC1=NC(Cl)=NC(Cl)=N1 MGNCLNQXLYJVJD-UHFFFAOYSA-N 0.000 description 4
- 230000006866 deterioration Effects 0.000 description 4
- 238000005286 illumination Methods 0.000 description 4
- 125000001160 methoxycarbonyl group Chemical group [H]C([H])([H])OC(*)=O 0.000 description 4
- 238000013508 migration Methods 0.000 description 4
- 230000005012 migration Effects 0.000 description 4
- 239000012074 organic phase Substances 0.000 description 4
- 235000019260 propionic acid Nutrition 0.000 description 4
- 238000000746 purification Methods 0.000 description 4
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 4
- 150000003254 radicals Chemical class 0.000 description 4
- 239000005060 rubber Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- 150000001412 amines Chemical class 0.000 description 3
- 229920005549 butyl rubber Polymers 0.000 description 3
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 3
- 238000004440 column chromatography Methods 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- 125000003386 piperidinyl group Chemical group 0.000 description 3
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 3
- 125000006239 protecting group Chemical group 0.000 description 3
- 230000035484 reaction time Effects 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 229920001897 terpolymer Polymers 0.000 description 3
- BMVXCPBXGZKUPN-UHFFFAOYSA-N 1-hexanamine Chemical compound CCCCCCN BMVXCPBXGZKUPN-UHFFFAOYSA-N 0.000 description 2
- 238000001644 13C nuclear magnetic resonance spectroscopy Methods 0.000 description 2
- 238000005160 1H NMR spectroscopy Methods 0.000 description 2
- CTZIWUMXEISMIY-UHFFFAOYSA-N C(C)(C)(C)C=1C=C(CCCOP(OCC)(O)=O)C=C(C1O)C(C)(C)C Chemical group C(C)(C)(C)C=1C=C(CCCOP(OCC)(O)=O)C=C(C1O)C(C)(C)C CTZIWUMXEISMIY-UHFFFAOYSA-N 0.000 description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 229920013649 Paracril Polymers 0.000 description 2
- 125000001797 benzyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])* 0.000 description 2
- 210000000481 breast Anatomy 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000007385 chemical modification Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 239000000806 elastomer Substances 0.000 description 2
- VAUPBJOFUFKEHV-UHFFFAOYSA-N hexane-1,1-diamine piperidine Chemical class N1CCCCC1.C(CCCCC)(N)N VAUPBJOFUFKEHV-UHFFFAOYSA-N 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 2
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000010534 nucleophilic substitution reaction Methods 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000003381 stabilizer Substances 0.000 description 2
- KZNICNPSHKQLFF-UHFFFAOYSA-N succinimide Chemical compound O=C1CCC(=O)N1 KZNICNPSHKQLFF-UHFFFAOYSA-N 0.000 description 2
- MFPWEWYKQYMWRO-UHFFFAOYSA-N tert-butyl carboxy carbonate Chemical compound CC(C)(C)OC(=O)OC(O)=O MFPWEWYKQYMWRO-UHFFFAOYSA-N 0.000 description 2
- 125000005931 tert-butyloxycarbonyl group Chemical group [H]C([H])([H])C(OC(*)=O)(C([H])([H])[H])C([H])([H])[H] 0.000 description 2
- 238000002834 transmittance Methods 0.000 description 2
- 125000004044 trifluoroacetyl group Chemical group FC(C(=O)*)(F)F 0.000 description 2
- 125000002221 trityl group Chemical group [H]C1=C([H])C([H])=C([H])C([H])=C1C([*])(C1=C(C(=C(C(=C1[H])[H])[H])[H])[H])C1=C([H])C([H])=C([H])C([H])=C1[H] 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 125000003088 (fluoren-9-ylmethoxy)carbonyl group Chemical group 0.000 description 1
- YQTCQNIPQMJNTI-UHFFFAOYSA-N 2,2-dimethylpropan-1-one Chemical group CC(C)(C)[C]=O YQTCQNIPQMJNTI-UHFFFAOYSA-N 0.000 description 1
- QIJIUJYANDSEKG-UHFFFAOYSA-N 2,4,4-trimethylpentan-2-amine Chemical compound CC(C)(C)CC(C)(C)N QIJIUJYANDSEKG-UHFFFAOYSA-N 0.000 description 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000004902 Softening Agent Substances 0.000 description 1
- 239000002174 Styrene-butadiene Substances 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 125000002252 acyl group Chemical group 0.000 description 1
- BHELZAPQIKSEDF-UHFFFAOYSA-N allyl bromide Chemical compound BrCC=C BHELZAPQIKSEDF-UHFFFAOYSA-N 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- HSDAJNMJOMSNEV-UHFFFAOYSA-N benzyl chloroformate Chemical compound ClC(=O)OCC1=CC=CC=C1 HSDAJNMJOMSNEV-UHFFFAOYSA-N 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
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- 230000000694 effects Effects 0.000 description 1
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- 230000002708 enhancing effect Effects 0.000 description 1
- 125000003754 ethoxycarbonyl group Chemical group C(=O)(OCC)* 0.000 description 1
- 230000005281 excited state Effects 0.000 description 1
- 125000003983 fluorenyl group Chemical class C1(=CC=CC=2C3=CC=CC=C3CC12)* 0.000 description 1
- 230000005283 ground state Effects 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical group 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- CXHHBNMLPJOKQD-UHFFFAOYSA-M methyl carbonate Chemical compound COC([O-])=O CXHHBNMLPJOKQD-UHFFFAOYSA-M 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000007344 nucleophilic reaction Methods 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- AICOOMRHRUFYCM-ZRRPKQBOSA-N oxazine, 1 Chemical compound C([C@@H]1[C@H](C(C[C@]2(C)[C@@H]([C@H](C)N(C)C)[C@H](O)C[C@]21C)=O)CC1=CC2)C[C@H]1[C@@]1(C)[C@H]2N=C(C(C)C)OC1 AICOOMRHRUFYCM-ZRRPKQBOSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000036961 partial effect Effects 0.000 description 1
- 125000000612 phthaloyl group Chemical group C(C=1C(C(=O)*)=CC=CC1)(=O)* 0.000 description 1
- 238000002464 physical blending Methods 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920000671 polyethylene glycol diacrylate Polymers 0.000 description 1
- 238000012667 polymer degradation Methods 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 1
- 235000015320 potassium carbonate Nutrition 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- CAEWJEXPFKNBQL-UHFFFAOYSA-N prop-2-enyl carbonochloridate Chemical compound ClC(=O)OCC=C CAEWJEXPFKNBQL-UHFFFAOYSA-N 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 239000003223 protective agent Substances 0.000 description 1
- 239000002516 radical scavenger Substances 0.000 description 1
- 206010037844 rash Diseases 0.000 description 1
- 239000003566 sealing material Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
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- 238000011105 stabilization Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 229960002317 succinimide Drugs 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 description 1
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- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention provides a polypropylene material and a preparation method for the polypropylene material. The polypropylene material is prepared in parts in weight: mixing 100 parts of polypropylene resin, 30-80 parts of flexibilizer, 2-4 parts of ethylene based multifunctional group monomer, 1.5-2.5 parts of hindered amine compound of a structure in a formula (I) and 0.15-0.25 parts of antioxygen, extruding, prilling and irradiating. Compared with a modified mode of mixing a light stabilizer and the polypropylene material in the prior art, the polypropylene material uses a modified mode that the hindered amine compound of the structure in the formula (I) serves as the light stabilizer to be mixed with the polypropylene material for irradiation. Firstly, the hindered amine compound contains end alkenyl groups with an unsaturated bond, and the hindered amine compound can be grafted on a macromolecule chain, so that the light stabilizer is not easy to move to a surface of the material; and secondly, modification is carried out by using irradiation, so that the material can form a three-dimensional space grid structure through crosslinking to limit movement of a molecular chain at the high temperature so as to improve heat-resistant property of the material.
Description
Technical field
The invention belongs to technical field of polymer materials, relate in particular to a kind of polypropylene material and preparation method thereof.
Background technology
Vestolen PP 7052 is the macromolecular compound that is obtained through polymerization by propylene, compares with other interchangeable heat thermoplastic plastics, has abundant raw material, cheap, advantage such as specific density is little, proof stress, resistance to chemical attack, wear resistance are good.And; Good, the easy processing of the mechanics equalization performance of polypropylene material, resistance to impact shock, resistance to flexing and electrical insulating property are good; Be the best product of thermotolerance in the resins for universal use, be widely used in conventional fields such as daily necessities, textiles, automobile component and the manufacturing of part medical apparatus.No matter Vestolen PP 7052 on output and consumption, still sees from its existing performance, one of the most promising material in the plastics beyond doubt.But Vestolen PP 7052 contains unsettled tertiary carbon group, is vulnerable to heat, oxygen and ultraviolet attack and the bad change of performance takes place, like xanthochromia, check surface and efflorescence; Mechanical property descends significantly; And along with the prolongation in storage time, polyacrylic degraded meeting sustainable development is until losing use value.Therefore, many products all propose the requirement of long-term illumination aging resisting performance modification to Vestolen PP 7052.
Polypropylene modification can be divided into chemical modification and two kinds of methods of physically modified.Chemical modification mainly is through copolymerization, grafting, mode such as crosslinked, changes polyacrylic molecular structure to reach the purpose of modification; Chemical reaction does not then take place in physically modified in whole process; In polypropylene matrix, add inorganic materials, organic materials, other plastics, rubber, thermoplastic elastomer or the interpolation auxiliary agent etc. of specific function is arranged, make PP composite material with excellent properties through means such as blend, enhancing or fillings.
At present; The illumination aging resisting performance modification of polypropylene material; Mainly be through adding various photostabilizers and heat-proof aging auxiliary agent and utilize two kinds of synergies between auxiliary agent to realize, and photostabilizer and heat-proof aging auxiliary agent are directly to be scattered in the material system through blend.But most of light stabilization aid comprises that various photomask agent, UV light absorber, radical scavenger etc. all are lower organic cpds of molecular weight or oligopolymer, and its speed to the material surface migration is very fast.When these auxiliary agents are added in the Vestolen PP 7052, under the situation of high temperature or UV-irradiation, the trend of separating out to product surface is gradually arranged all.
Application number is that the Chinese patent of CN96197212.2 discloses a kind of radiation tolerant polypropylene and product thereof; Vestolen PP 7052 by 50% ~ 99% and 1% ~ 50% polyethylene blend add the anti-irradiation transparent polypropylenes of preparation such as hindered amine stabilizer, auxiliary antioxidant and nucleator.Only through the method for physical blending, it is easy to move to material surface in the interpolation of stablizer; And hindered amine stabilizer is soluble in the organic solvent such as methylcarbonate,, also can be dissolved in solvent to separate out during as the photostabilizer life-time service of sealing material with it, causes the illumination aging resisting performance of material to descend.
Summary of the invention
In view of this, the technical problem that the present invention will solve is to provide a kind of polypropylene material and preparation method thereof, and the illumination aging resisting performance of this polypropylene material is better.
The invention provides a kind of polypropylene material, mainly behind blend, irradiation, prepare by following raw material:
Acrylic resin 100 weight parts;
Toughner 30 ~ 80 weight parts;
Vinyl polyfunctional monomer 2 ~ 4 weight parts;
Hindered amine compound 1.5 ~ 2.5 weight parts of formula (I) structure;
Oxidation inhibitor 0.15 ~ 0.25 weight part;
Wherein, m=1 ~ 9, n=3 ~ 10.
Preferably, said inhibitor is 3,5-di-tert-butyl-4-hydroxyl benzyl diethyl phosphoric acid or β-(4-hydroxyl-3,5-di-tert-butyl-phenyl) positive octadecyl ester of propionic acid.
Preferably, said vinyl polyfunctional monomer is trivinyl polyfunctional monomer or divinyl polyfunctional monomer.
Preferably, said trivinyl polyfunctional monomer is Viscoat 295, pentaerythritol triacrylate or cyanacrylate.
Preferably, said divinyl polyfunctional monomer is polyethyleneglycol diacrylate or PDDA.
Preferably, said toughner is TPR.
Preferably, said TPR is POE, styrene-butadiene-styrene multipolymer, hydrogenated styrene-butadiene-styrene multipolymer, terpolymer EP rubber, tree elastomer, styrene-butadiene rubber(SBR), paracril or butyl rubber.
The invention provides a kind of preparation method of polypropylene material, may further comprise the steps:
The hindered amine compound of formula (I) structure of the vinyl polyfunctional monomer of the toughner of the acrylic resin of 100 weight parts, 30 ~ 80 weight parts, 2 ~ 4 weight parts, 1.5 ~ 2.5 weight parts is mixed with the inhibitor of 0.15 ~ 0.25 weight part; Extruding pelletization obtains polypropylene material behind the irradiation;
Wherein, m=1 ~ 9, n=3 ~ 10.
Preferably, the temperature of said extruding pelletization is 180 ℃ ~ 200 ℃.
Preferably, the radiation dose rate of said irradiation is 1000 ~ 5000rad/min, and irradiation dose is 5 ~ 30kGy.
The invention provides a kind of polypropylene material and preparation method thereof; This polypropylene material raw material comprises hindered amine compound and the oxidation inhibitor of 0.15 ~ 0.25 weight part of formula (I) structure of vinyl polyfunctional monomer, 1.5 ~ 2.5 weight parts of toughner, 2 ~ 4 weight parts of acrylic resin, 30 ~ 80 weight parts of 100 weight parts; Raw materials mix obtains polypropylene material through extruding pelletization after the radiation.Directly carry out modification with the polypropylene material blend with the prior art photostabilizer and compare, it is that photostabilizer and polypropylene material blend are after radiation modification that the present invention utilizes the hindered amine compound of formula (I) structure.At first, the hindered amine compound of formula (I) structure contains the end alkenyl group of unsaturated link(age), can it be grafted on the macromolecular chain through irradiation technique; Form carbon-carbon bond; Therefore photostabilizer is difficult for to the material surface migration, also is difficult for dissolving and separates out, and the light stability of material strengthens; Secondly, the method for employing irradiation is carried out modification also can make material through being cross-linked to form the three-dimensional space grid structure, has limited molecular chain motion at high temperature, thereby improves the resistance toheat of polypropylene material.
Experimental result shows, polypropylene material of the present invention behind accelerated light ageing tensile strength of material, modulus in flexure and normal temperature IZOD notched Izod impact strength retention all greater than 80%.
Embodiment
The invention provides a kind of polypropylene material; Mainly by following feedstock production: the acrylic resin of 100 weight parts; The toughner of 30 ~ 80 weight parts; The vinyl polyfunctional monomer of 2 ~ 4 weight parts, the hindered amine compound of the formula of 1.5 ~ 2.5 weight parts (I) structure and the oxidation inhibitor of 0.15 ~ 0.25 weight part.
In the formula (I), m=1 ~ 9, n=3 ~ 10.M is preferably 1 ~ 6, and more preferably 2 ~ 4.
Wherein, said toughner is preferably 40 ~ 80 weight parts, more preferably 50 ~ 70 weight parts.Said toughner is preferably TPR; More preferably POE (POE), styrene-butadiene-styrene multipolymer (SBS), hydrogenated styrene-butadiene-styrene multipolymer (SEBS), terpolymer EP rubber (EPDM), tree elastomer (NR), styrene-butadiene rubber(SBR) (SBR), paracril (NBR) or butyl rubber (IR) are preferably POE, styrene-butadiene-styrene multipolymer, terpolymer EP rubber or butyl rubber again.Toughner and the polypropene blended low-temperature impact toughness that can improve polypropylene material.
Said vinyl polyfunctional monomer is preferably 2.5 ~ 4 weight parts, more preferably 2.5 ~ 3.5 weight parts.Said vinyl polyfunctional monomer is preferably trivinyl polyfunctional monomer or divinyl polyfunctional monomer.Said trivinyl polyfunctional monomer is preferably Viscoat 295 (TMPTA), pentaerythritol triacrylate (PETA) or cyanacrylate (TAIC), more preferably Viscoat 295 or cyanacrylate; Said divinyl polyfunctional monomer is preferably polyethyleneglycol diacrylate (PEGDA) or PDDA (PDDA), more preferably PDDA.Because polypropylene material is degraded easily under radiation parameter; And the vinyl polyfunctional monomer can impel polypropylene material crosslinked; Therefore the use of vinyl polyfunctional monomer can reduce the used dosage of irradiation, suppresses the degraded and the performance degradation of polypropylene material to a certain extent.
The hindered amine compound of said formula (I) structure is preferably 1.5 ~ 2.2 weight parts; 1.5 ~ 2 weight parts more preferably, it contains the end alkenyl group of unsaturated link(age), can it be grafted on the macromolecular chain through irradiation technique; Form carbon-carbon bond; Photostabilizer is difficult for to the material surface migration, also is difficult for separating out, improved the resistance to light of polypropylene material because of being dissolved in organic solvent.
Said oxidation inhibitor is preferably 0.15 ~ 0.22 weight part, more preferably 0.17 ~ 0.2 weight part.Said oxidation inhibitor is preferably 3,5-di-tert-butyl-4-hydroxyl benzyl diethyl phosphoric acid or β-(4-hydroxyl-3,5-di-tert-butyl-phenyl) positive octadecyl ester of propionic acid.
The present invention also provides the preparation method of above-mentioned polypropylene material; May further comprise the steps: the hindered amine compound of formula (I) structure of the vinyl polyfunctional monomer of the toughner of the acrylic resin of 100 weight parts, 30 ~ 80 weight parts, 2 ~ 4 weight parts, 1.5 ~ 2.5 weight parts and the inhibitor of 0.15 ~ 0.25 weight part are mixed; Add blend granulation in the twin screw extruder; Extrusion temperature is 180 ℃ ~ 200 ℃, is preferably 190 ℃ ~ 200 ℃, obtains polypropylene material behind the irradiation.
According to the present invention, the masterbatch that said extruding pelletization obtains preferably dry to moisture content less than 1.5 ‰, afterwards, carry out irradiation.The irradiation source of said irradiation is an irradiation source well known to those skilled in the art, preferably adopts the Co-60 source.The radiation dose rate of said irradiation is 1000 ~ 5000rad/min, is preferably 2000 ~ 4500rad/min, 2500 ~ 4000rad/min more preferably, and radiation dose rate is 5 ~ 30kGy, is preferably 10 ~ 30kGy, more preferably 10 ~ 20kGy.
Traditional blend method can cause the significantly sacrificing of other aspect performances usually when improving some performance of polypropylene material, wherein relatively more outstanding is exactly the balance between polypropylene material low-temperature flexibility and the resistance toheat.Adopt the method for blend softening agent that the low-temperature flexibility of polypropylene material is carried out modification among the present invention; Utilize irradiation to carry out modification then; Behind irradiation; Polypropylene material can be cross-linked to form the three-dimensional space grid structure, thus the motion at high temperature of restriction molecule chain, the resistance toheat of raising polypropylene material.Simultaneously; Forming chemical bond between the hindered amine compound that also makes photostabilizer formula (I) structure through irradiation and macromolecular chain is connected; Photostabilizer is difficult for to the material surface migration, also is difficult for separating out, improved the resistance to light of polypropylene material because of being dissolved in organic solvent.
Wherein, the hindered amine compound of said formula (I) structure preferably prepares according to following steps: A) compound with formula (II) structure reacts in protective atmosphere with protection reagent, obtains the intermediate product of amido protecting; B), obtain the hindered amine compound of formula (I) structure behind the deprotection with the intermediate product of said amido protecting and the end ene compound reaction of formula (III) structure.Said protective atmosphere is a protective atmosphere well known to those skilled in the art, is preferably nitrogen.
Wherein, m=1 ~ 9, n=310, X are Cl, Br or I.M is preferably 1 ~ 6, and more preferably 2 ~ 4.
The compound of said formula (II) structure is that model well known to those skilled in the art is the photostabilizer of GW-944.
In the steps A, the compound of said formula (II) structure is 1:2 ~ 2.5 with the mol ratio of protection reagent, is preferably 1:2 ~ 2.2.The reaction times of said reaction is 3.5 ~ 4.5h.The amount of substance and the reaction times of control protection reagent, make and have only two amino on the piperidine ring to be protected among the GW-944.Said steps A reaction is preferably carried out in organic solvent, and said organic solvent is an organic solvent well known to those skilled in the art, is preferably methylene dichloride.
Said blocking group is carbalkoxy class amido protecting group, acyl group class amido protecting group or alkyls amido protecting group.Follow the principle that is prone to quilt protection and easy deprotection and select blocking group, said blocking group is preferably carbalkoxy class amido protecting group.
Said carbalkoxy class amido protecting group is preferably carbobenzoxy-(Cbz), tertbutyloxycarbonyl, tablet held before the breast by officials methoxycarbonyl, allyloxycarbonyl, trimethylsilyl ethoxycarbonyl, methoxycarbonyl or ethoxycarbonyl, more preferably tertbutyloxycarbonyl (Boc) or tablet held before the breast by officials methoxycarbonyl (Fmoc).
Said acyl group class amido protecting group is preferably phthaloyl, p-toluenesulfonyl, trifluoroacetyl group, ortho-nitrophenyl alkylsulfonyl, p-nitrophenyl alkylsulfonyl, pivaloyl group or benzoyl-, more preferably p-toluenesulfonyl or trifluoroacetyl group.
Said alkyls amido protecting group is preferably trityl, 2,4-dimethoxy-benzyl, to methoxy-benzyl or benzyl, more preferably trityl or benzyl.
The selection of blocking group affects the selection of deprotection reaction condition in the protective reaction and step B in the steps A, adopts the condition opposite with protective reaction pH value to carry out deprotection.Can select corresponding protection reagent according to blocking group, said protection reagent is preferably amido protecting agents such as tert-Butyl dicarbonate, chloroformic acid benzyl ester, chloroformic acid-9-fluorenyl methyl esters, fluorenes methoxy carbonyl acyl succinimide or allyl chlorocarbonate.
The intermediate product of the amido protecting that obtains in the steps A need not to separate purification, and the end ene compound that can directly add formula (III) structure carries out next step reaction.
According to the present invention, the mol ratio of the end ene compound of the intermediate product of amido protecting and formula (III) structure is 1:1 ~ 4 among the said step B, be preferably 1: 1 ~ and 3, more preferably 1: 1.5 ~ 2.2.
The reaction times of the end ene compound of the intermediate product of amido protecting and formula (III) structure reaction is 9 ~ 15h among the said step B.The product that obtains behind the deprotection obtains the hindered amine compound of pure formula (I) structure through purification step, and said purification step is preferably column chromatography for separation and purifies, and more preferably the mixed solution of normal hexane and ETHYLE ACETATE carries out the column chromatography for separation purification.
Among the present invention; After utilizing blocking group that the amino on the piperidine ring is protected; The end ene compound is through terminal halogen and the not protected amino nucleophilic reaction that takes place; And then link to each other with GW-944, the unsaturated link(age) that wherein contains can be grafted to it on macromolecular chain through irradiation technique, forms carbon-carbon bond.
When using as photostabilizer; Generate NO free radical after the piperidine ring oxidation of hindered amine compound; NO free radical can make the singlet oxygen that is in excited state get back to ground state through transmitting the approach of energy, thereby stops singlet oxygen to cause the generation of polymer degradation reaction; Also further capturing free radicals of NO free radical simultaneously, the light stabilising effect of raising hindered amine compound.And hindered amine compound of the present invention is owing to link to each other with macromolecular material through chemical bond, so is not soluble in organic solvent and separates out, and light stability is strong.
According to the present invention, said GW-944 preferably prepares according to following steps: S1) cyanuric chloride and uncle's hexylamine are reacted in solvent, obtain the intermediate product of formula (IV) structure; S2) intermediate product and the hexanediamine piperidines with said formula (IV) structure reacts in protective atmosphere, obtains the GW-944 of formula (II) structure.Wherein, said solvent is an organic solvent well known to those skilled in the art, is preferably toluene.Said protective atmosphere is a protective atmosphere well known to those skilled in the art, is preferably nitrogen.
The temperature of reaction of said step S1 is 0 ℃ ~ 10 ℃.Three chlorine atomic reaction activity of cyanuric chloride are all higher, and therefore facile hydrolysis need react at low temperatures.Cyanuric chloride and the reaction of uncle's hexylamine produce HCl, need to add acid binding agent and improve speed of reaction, and acid binding agent described in the present invention is preferably the NaOH aqueous solution.
Said step S2 preferably reacts under the condition of acid binding agent, and said acid binding agent is preferably the NaOH aqueous solution.
Among the present invention, said step S2 is specially: S21) under 50 ℃ ~ 70 ℃ conditions, be preferably 55 ℃ ~ 65 ℃, reaction 3 ~ 5h, the intermediate product generation nucleophilic substitution reaction of quadrol piperidines and formula (IV) structure; S22) above-mentioned reaction system is warming up to 160 ℃ ~ 200 ℃, is preferably 170 ℃ ~ 185 ℃, reaction 5 ~ 7h, the product generation polycondensation of nucleophilic substitution obtains GW-944.
In order to further specify the present invention, a kind of hindered amine compound provided by the invention and preparation method thereof is described in detail below in conjunction with embodiment.
Agents useful for same is commercially available in following examples.
The preparation of embodiment 1GW-944
1.1 with being cooled to below 10 ℃ under the 120ml toluene condition of ice bath, add the 40g cyanuric chloride, stir; Slowly drip the toluene solution 50ml that is dissolved with the 27.52g tert-Octylamine, behind the reaction 2h, the dropping mass concentration is 20% NaOH aqueous solution 50ml; Reaction 2h leaves standstill, and tells organic phase; The use mass concentration is 10% NaOH solution washing, obtains containing the organic phase of intermediate product IV.
1.2 with the organic phase that contains 0.2mol intermediate product IV that obtains in 1.1,0.2mol hexanediamine piperidines and 50ml mass concentration are that 20% the NaOH aqueous solution adds in the 500ml autoclave, behind the air three times, inflated with nitrogen to pressure is 2MPa in the nitrogen replacement still; Be heated to 60 ℃, behind the stirring reaction 4h, be warming up to 180 ℃, reaction 6h; Cooling is filtered, and it is behind 10% the NaOH solution washing that organic phase is used mass concentration; Revolve to steam to remove and desolvate, get GW-944, average molecular mass is 2240.
Utilize transmittance/mist degree tester that the GW-944 that obtains in 1.2 is tested according to GB2410-80, obtain its transmittance T
425nm>96%, T
450nm>96%.
Utilize nucleus magnetic resonance respectively the GW-944 that obtains in 1.2 to be analyzed, obtain its hydrogen spectrum and compose with carbon, the result is following:
1HNMR（CDCl
3,ppm）：4.0(-NH),3.49(-CH
2),3.35(-CH
2),2.63(-CH),2.44(-CH),2.26(-CH),1.32(-NH),1.49-CH),1.31(-CH),0.94(-CH
3)。
13CNMR（CDCl
3,ppm）：180.7,176.5,160.4,61.1,54.5,51.5,45,42,39.7,29.5,29,22.7,14.1。
Embodiment 2
Under the condition of nitrogen protection, with the GW-944 that obtains among the 0.2mol 1.2, the 0.4mol tert-Butyl dicarbonate, 0.18mol salt of wormwood and 120ml methylene dichloride mix stirring, behind the reaction 4h, add the 0.3mol allyl bromide 98, continue reaction 10h.Adding Hydrogen chloride transfers to 5.0, removal of solvent under reduced pressure, extracted with diethyl ether, anhydrous Na with the pH value of reaction solution
2SO
4Drying obtains the hindered amine compound of formula (I) structure after the n-hexane/ethyl acetate column chromatography is purified, its average molecular mass is 2960.
Utilize nucleus magnetic resonance respectively the hindered amine compound of formula (I) structure that obtains among the embodiment 2 to be analyzed, obtain its hydrogen spectrum and compose with carbon, the result is following:
1HNMR（CDCl
3,ppm）：5.87(-C=CH),5.19(-C=CH),3.73(-CH
2),3.49(-CH
2),2.63(-CH),2.44(-CH),2.26(-CH),2.0(-NH),1.49-CH
2),1.32(-CH),0.94(-CH
3)。
13CNMR（CDCl
3,ppm）：180.7,177.1,134.2,117.1,61.1,54.5,51.5,45,42,39.7,29.5,29,22.7,14.1。
Embodiment 3
Hindered amine compound and 1.5g 3 with formula (I) structure that obtains among the 1000g Vestolen PP 7052 of drying, 300g POE, 30g TMPTA, the 15g embodiment 2; 5-di-tert-butyl-4-hydroxyl benzyl diethyl phosphoric acid mixes; Be added to blend granulation in the twin screw extruder, extrusion temperature is 180 ℃ ~ 200 ℃, and head temperature is 190 ℃; The material of extruding pelletizing after the running water cooling obtains masterbatch; Masterbatch is dried to water cut less than after 1.5 ‰, uses Co-60 source irradiation in a vacuum, and dose rate is 1000rad/min, and total absorption dose is 5kGy, obtains polypropylene material.
Tensile strength, modulus in flexure, shock strength, vicat softening temperature and gel content according to the polypropylene material that obtains among 2546 couples of embodiment 3 of GB/T are tested, and the test result that obtains is as shown in table 1.
The mechanical property of material is tested after utilizing the UV-light accelerated deterioration to the polypropylene material accelerated light ageing that obtains among the embodiment 3, and the ultraviolet lighting total dose is 7.7 * 10
6Rad obtains the mechanical property retention of material behind its accelerated light ageing, and is as shown in table 2.
Embodiment 4
Hindered amine compound and 1.5g β-(4-hydroxyl-3 with formula (I) structure that obtains among the 1000g Vestolen PP 7052 of drying, 500g SBS, 20g TMPTA, the 18g embodiment 2; The 5-di-tert-butyl-phenyl) the positive octadecyl ester of propionic acid mixes; Be added to blend granulation in the twin screw extruder, extrusion temperature is 180 ℃ ~ 200 ℃, and head temperature is 190 ℃; The material of extruding pelletizing after the running water cooling obtains masterbatch; Masterbatch is dried to water cut less than after 1.5 ‰, uses Co-60 source irradiation in a vacuum, and dose rate is 5000rad/min, and total absorption dose is 10kGy, obtains polypropylene material.
Tensile strength, modulus in flexure, shock strength, vicat softening temperature and gel content according to the polypropylene material that obtains among 2546 couples of embodiment 4 of GB/T are tested, and the test result that obtains is as shown in table 1.
The mechanical property of material is tested after utilizing the UV-light accelerated deterioration to the polypropylene material accelerated light ageing that obtains among the embodiment 4, and the ultraviolet lighting total dose is 7.7 * 10
6Rad obtains the mechanical property retention of material behind its accelerated light ageing, and is as shown in table 2.
Embodiment 5
Hindered amine compound and 2g 3 with formula (I) structure that obtains among the 1000g Vestolen PP 7052 of drying, 600g SBS, 25g TAIC, the 20g embodiment 2; 5-di-tert-butyl-4-hydroxyl benzyl diethyl phosphoric acid mixes; Be added to blend granulation in the twin screw extruder, extrusion temperature is 180 ℃ ~ 200 ℃, and head temperature is 190 ℃; The material of extruding pelletizing after the running water cooling obtains masterbatch; Masterbatch is dried to water cut less than after 1.5 ‰, uses Co-60 source irradiation in a vacuum, and dose rate is 3000rad/min, and total absorption dose is 15kGy, obtains polypropylene material.
Tensile strength, modulus in flexure, shock strength, vicat softening temperature and gel content according to the polypropylene material that obtains among 2546 couples of embodiment 5 of GB/T are tested, and the test result that obtains is as shown in table 1.
The mechanical property of material is tested after utilizing the UV-light accelerated deterioration to the polypropylene material accelerated light ageing that obtains among the embodiment 5, and the ultraviolet lighting total dose is 7.7 * 10
6Rad obtains the mechanical property retention of material behind its accelerated light ageing, and is as shown in table 2.
Embodiment 6
Hindered amine compound and 2.5g β-(4-hydroxyl-3 with formula (I) structure that obtains among the 1000g Vestolen PP 7052 of drying, 800g IR, 40g PDDA, the 22g embodiment 2; The 5-di-tert-butyl-phenyl) the positive octadecyl ester of propionic acid mixes; Be added to blend granulation in the twin screw extruder, extrusion temperature is 180 ℃ ~ 200 ℃, and head temperature is 190 ℃; The material of extruding pelletizing after the running water cooling obtains masterbatch; Masterbatch is dried to water cut less than after 1.5 ‰, uses Co-60 source irradiation in a vacuum, and dose rate is 4100rad/min, and total absorption dose is 30kGy, obtains polypropylene material.
Tensile strength, modulus in flexure, shock strength, vicat softening temperature and gel content according to the polypropylene material that obtains among 2546 couples of embodiment 6 of GB/T are tested, and the test result that obtains is as shown in table 1.
The mechanical property of material is tested after utilizing the UV-light accelerated deterioration to the polypropylene material accelerated light ageing that obtains among the embodiment 6, and the ultraviolet lighting total dose is 7.7 * 10
6Rad obtains the mechanical property retention of material behind its accelerated light ageing, and is as shown in table 2.
The partial properties of table 1 polypropylene material
Material mechanical performance retention behind table 2 accelerated light ageing
The above only is a preferred implementation of the present invention; Should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention; Can also make some improvement and retouching, these improvement and retouching also should be regarded as protection scope of the present invention.
Claims (10)
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